Increasing awareness concerning food safety problems has been driving the search for simple and efficient biochemical analytical methods.In this paper,we develop a portable electro-acoustic biosensor based on a film b...Increasing awareness concerning food safety problems has been driving the search for simple and efficient biochemical analytical methods.In this paper,we develop a portable electro-acoustic biosensor based on a film bulk acoustic resonator for the detection of pesticide residues in agricultural products.A shear mode ZnO film bulk acoustic resonator with a micro-machining structure was fabricated as a mass-sensitive transducer for the real-time detection of antibody-antigen reactions in liquids.In order to obtain an ultra-low detection level,the artificial antigens were immobilized on the sensing surface of the resonator to employ a competitive format for the immunoassays.The competitive immunoreactions can be observed clearly through monitoring the frequency changes.The presence of pesticides was detected through the diminution of the frequency shift compared with the level without pesticides.The limit of detection for carbaryl(a widely used pesticide for vegetables and crops)is2?10-10 M.The proposed device represents a potential alternative to the complex optical systems and electrochemical methods that are currently being used,and represents a significant opportunity in terms of simplicity of use and portability for on-site food safety testing.展开更多
The QuEChERS extraction technique is a pretreatment technique that has been rapidly applied in recent years and is widely used in the field of pesticide residues with many advantages. This technique is based on solid ...The QuEChERS extraction technique is a pretreatment technique that has been rapidly applied in recent years and is widely used in the field of pesticide residues with many advantages. This technique is based on solid phase extraction (SPE), which uses the interaction between adsorbent and impurities in the matrix to achieve the purpose of purification. The method has easier operation and better purification effect than SPE. In this paper, the research progress of the QuEChERS technique in pesticide residue detection in different fields in recent years and its future development were reviewed, hoping to provide reference for further development and utilization of the QuEChERS technique in pesticide residue detection in the future.展开更多
[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by ga...[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry(GC-MS)in selective ion scanning mode(SIM).[Results]The organophosphorus pesticide standard solutions showed good linearity in the mass concentration range of 0.1-10.0μg/ml with correlation coefficients(r)not lower than 0.999,and the detection limits(S=3 N)ranged from 0.01 to 0.05 mg/kg.The average recovery values were in the range of 80.2%-99.7%,with relative standard deviations(RSDs,n=3)in the range of 1.8%-6.3%,at the addition levels of 0.5,1.0 and 2.0 mg/kg.[Conclusions]The method is simple,sensitive and accurate,and can be used for the determination of organophosphorus pesticide residues in mutton.展开更多
Pesticide residues treatment is a crucial issue for both agricultural production and environmental protection.In recent years,designing self-cleaning nanoformulations has emerged as a promising strategy for reducing p...Pesticide residues treatment is a crucial issue for both agricultural production and environmental protection.In recent years,designing self-cleaning nanoformulations has emerged as a promising strategy for reducing pesticide residues in a convenient and cost-effective manner.However,traditional physical blending methods of photodegradation reagents with nanocarriers have limitations in terms of pesticide residue degradation efficiency and active ingredient efficacy.Here,a new type of timing self-cleaning nanoherbicide dicamba@mSiO_(2)/ATA/TiO_(2)with a triple structure was fabricated.Dicamba,a widely used herbicide that was attracting increasing concern over its high efficiency and broad spectrum,was selected as the model herbicide and loaded on the mSiO_(2)shell.In the stage of pesticide release,the TiO_(2)and dicamba were separated by the timing-barrier.Therefore,the efficacy of dicamba was not affected by the photocatalyst.During the release process,the ATA layer continuously absorbed the reactive oxygen species(ROS)produced by TiO_(2)and was gradually degraded.Finally,the barrier was destroyed,and the residual dicamba in the carrier was degraded by TiO_(2).Compared with the traditional physical blending method,this triple structure avoided the degradation of active ingredients by photocatalysts during the pesticide release period.The experimental results suggested that this nanoformulation improved the efficacy of the herbicide,and reduced the pesticide residues,providing a new approach for self-cleaning nanopesticides research.展开更多
[Objective] The aim was to explore the application of terahertz （THz） technique in pesticide recognition and residue determination. [Method] THz far-infrared spectral characteristics of 2 herbicides （butachlor and ...[Objective] The aim was to explore the application of terahertz （THz） technique in pesticide recognition and residue determination. [Method] THz far-infrared spectral characteristics of 2 herbicides （butachlor and metolachlor） were measured by THz time-domain spectroscopy （THz-TDS） under conditions of room temperature and nitrogen,meanwhile their refractive index and absorption coefficient between 0.2 and 2.2 THz were calculated by using models based on Fresenl equations. [Result] The 2 pesticides both had a series of different characteristic absorption peaks between 0.2 and 2.2 THz,respectively. Their molecular structures were similar,but there were great difference in absorption and refractive index spectrum between them. [Conclusion] THz-TDS technique is feasible to detect pesticide residues,especially there is a greater advantage in identifying the structure of similar substances.展开更多
[Objective] This study was conducted to develop a system for simultaneous determination of imidacloprid, diflubenzuron, thiabendazole and carbendazim in fruit juice by HPLC. [Method] Using acetonitrile as the extracti...[Objective] This study was conducted to develop a system for simultaneous determination of imidacloprid, diflubenzuron, thiabendazole and carbendazim in fruit juice by HPLC. [Method] Using acetonitrile as the extraction solvent, the pesticides in fruit juice were purified through a NH2 solid phase extraction （SPE） cartridge, then detected by HPLC. [Result] There was a good linear relationship between the peak area and the concentrations of imidacloprid, diflubenzuron, thiabendazole and carbendazim in a range of 0.05-5.0 μg/ml, and the linear correlation coefficient varied in a range of 0.999 0-0.999 8; the limit of detection for imidacloprid, diflubenzuron, thiabendazole and carbendazim was 0.003, 0.005, 0.003 and 0.007 mg/kg, respectively. The recovery rate of imidacloprid, diflubenzuron, thiabendazole and carbendazim standards added at three levels （0.1, 0.5 and 1.0 mg/kg） ranged from 82% to 107%, with RSD less than 4.5%. [Conclusion] The sensitivity, accuracy and precision of this method were able to meet the requirements for pesticide residue analysis.展开更多
[Objective] A method was developed for the determination of 10 pyrethroids pesticide residues in rice by GC-MS-MS. [Method] Pyrethroids were extracted with acetonitrile, followed by a salting-out step with anhydrous m...[Objective] A method was developed for the determination of 10 pyrethroids pesticide residues in rice by GC-MS-MS. [Method] Pyrethroids were extracted with acetonitrile, followed by a salting-out step with anhydrous magnesium sulfate and sodium chloride, cleaned up by florisil solid phase extraction （SPE） cartridge, and determined by multiple reaction monitoring mode. [Result] The method showed good linearity over the range of 0.010-0.500 mg/L for 10 pyrethroid pesticide with correlation coefficients over 0.99. The detection limits were 0.005 -0.010 mg/kg. The method was validated by analyzing samples spiked with 0.05, 0.10, 0.20 mg/kg of 10 pyrethroid pesticides, respectively. The average recoveries in rice ranged from 75.0-115.5%, and the relative standard deviations （RSD） were between 3.9%-6.9%. [Conclusion] The method is easy, accurate and reliable, which can meet the requirement for the simultaneous determination and confirmation of pyrethroid pesticide residues in rice.展开更多
The analysis of pesticide residues in Citrus from Yichang, Danjiangkou, Zigui and Xingshan in Hubei Province was accomplished by UPLC-MS and GC-MS. The results showed that the detection rate of pesticide residues in C...The analysis of pesticide residues in Citrus from Yichang, Danjiangkou, Zigui and Xingshan in Hubei Province was accomplished by UPLC-MS and GC-MS. The results showed that the detection rate of pesticide residues in Citrus reticulate was 91.9%. The detection rate of banned pesticides was 1.6%. The detection rate of restricted pesticides was 9.5%. The detection rate of allowed pesticides was 68.3%. The detection rate of unregistered pesticides was 15.9%. The pesticide used in citrus was relatively common. Because of the banned and restricted pesticides were both in the control degree, on the whole, the quality and security of Citrus reticulata was safe.展开更多
In order to study the difference between cauliflower varieties with ball well protected and unprotected in terms of pesticide residue and its causes, Jinpin 70, a new male sterile cauliflower variety with ball well pr...In order to study the difference between cauliflower varieties with ball well protected and unprotected in terms of pesticide residue and its causes, Jinpin 70, a new male sterile cauliflower variety with ball well protected, and Xuebao with ball unprotected were sprayed with high-toxic pesticide phorate and efficient bio-pesticide emamectin benzoate at a regular dose to investigate the impact of different cauliflower varieties on the pesticide residue. The results showed that from the 3rd to the 5th day after spraying, phorate and emamectin benzoate residues in Jinpin 70 with ball well protected reduced by 76.47%-87.65% and 67.86%-80.82% re- spectively compared with Xubao, and decreased by 9.23%-81.82% and 57.14%- 79.84% respectively compared with Jinpin 70 with ball unprotected. The results above demonstrates that inner leaves of cauliflower with ball well protected can prevent the ball from being polluted by phorate and emamectin benzoate, thereby improving its edible safety.展开更多
The pretreatment and analytical techniques for organochiorine residues, including ultrasonic extraction, accelerated solvent extraction pesticide microwave extraction, solid phase extraction, and solid-phase micro-ext...The pretreatment and analytical techniques for organochiorine residues, including ultrasonic extraction, accelerated solvent extraction pesticide microwave extraction, solid phase extraction, and solid-phase micro-extraction and the analytical techniques of gas chromatography and gas chromatography-mass spectrometry）in tea samples in recent years were reviewed. The prospect of organochlorine pesti- cide residue analysis was proposed in this paper.展开更多
This study was aimed to do the prediction of pesticide residues based on fuzzy system. Taking chlorpyrifos as an example, the Mathematic Fuzzy System was established by using the MRL values （maximum residue limits of...This study was aimed to do the prediction of pesticide residues based on fuzzy system. Taking chlorpyrifos as an example, the Mathematic Fuzzy System was established by using the MRL values （maximum residue limits of all kinds of pesticides in food） of the Matlab Fuzzy Toolbox to analyze and predict the degra- dation degree of pesticide residues of the same crop at different time periods of bagging treatment, with the aim to provide some theoretical guidances for solving practical problems in real life.展开更多
A field study was conducted in the Taihu Lake region, China in 2004 to reveal the organochlorine pesticide concentrations in soils after the ban of these substances in the year 1983. Thirteen organochlorine pesticides...A field study was conducted in the Taihu Lake region, China in 2004 to reveal the organochlorine pesticide concentrations in soils after the ban of these substances in the year 1983. Thirteen organochlorine pesticides （OCPs） were analyzed in soils from paddy field, tree land and fallow land. Total organochlorine pesticide residues were higher in agricultural soils than in uncultivated fallow land soils. Among all the pesticides, ΣDDX （DDD, DDE and DDT） had the highest concentration for all the soil samples, ranging from 3.10 ng/g to 166.55 ng/g with a mean value of 57.04 ng/g and followed by ΣHCH, ranging from 0.73 ng/g to 60.97 ng/g with a mean value of 24.06 ng/g. Dieldrin, endrin, HCB and α-endosulfan were also found in soils with less than 15 ng/g. Ratios of p,p＇-（DDD＋DDE）/DDT in soils under three land usages were： paddy field 〉 tree land 〉 fallow land, indicating that land usage inlfuenced the degradation of DDT in soils. Ratios of p,p＇-（DDD＋DDE）/DDT 〉1, showing aged residues of DDTs in soils of the Taihu Lake region. The results were discussed with data from a former study that showed very low actual concentrations of HCH and DDT in soils in the Taihu Lake region, but according to the chemical half-lives and their concentrations in soils in 1980s, the concentration of DDT in soils seemed to be underestimated. In any case our data show that the ban on the use of HCH and DDT resulted in a tremendous reduction of these pesticide residues in soils, but there are still high amounts of pesticide residues in soils, which need more remediation processes.展开更多
To ensure the safety of the commercially available chenpi,a convenient and fast analytical method was developed for the determination of 133 pesticide residues in chenpi using gas chromatography-tandem mass spectromet...To ensure the safety of the commercially available chenpi,a convenient and fast analytical method was developed for the determination of 133 pesticide residues in chenpi using gas chromatography-tandem mass spectrometry(GC-MS/MS).In this study,different extraction solvents,redissolution solvents and adsorbents were tested according to the recovery and purification effect to obtain a modified QuEChERS method.The samples were extracted with acetonitrile.During the clean-up step,octadecyl-modified silica(C18)and graphitized carbon black(GCB)were selected,and aminopropyl(NH2)was used instead of primary secondary amine(PSA)because of its weaker ion exchange capacity which had little effect on the recovery of ditalimfos.Samples were quantified by matrix-matched calibration with internal standards.All pesticides showed good linearity in the respective range,both with values of r2>0.99.The average recoveries of the pesticides spiked samples ranged from 70.0% to 112.2% with the RSDs of 0.2%–14.4%.The modified QuEChERS method was validated and applied to twenty real samples.Five pesticides were found in eight batches,but no pesticide exceeded the maximum residue limits(MRL,MRL reference to European commission).展开更多
The presence of pesticide residues in pears is a serious health concern. This study presents the results from a 2-year investigation （2013-2014） that used gas chromatography, GS/MS and UPLC/MS-MS to measure the leve...The presence of pesticide residues in pears is a serious health concern. This study presents the results from a 2-year investigation （2013-2014） that used gas chromatography, GS/MS and UPLC/MS-MS to measure the levels of 104 pesti- cides in 310 pear samples. In 93.2% of the samples, 43 pesticides were detected, of which the maximum residue levels （MRLs） were exceeded in 2.6% of the samples. Multiple residues （two to eight compounds） were present in 69.7% of the samples; one sample contained nine pesticides and one sample contained 10. Only 6.8% of the samples did not contain residues. To assess the health risks, the pesticide residue data have been combined with daily pear consumption data for children and adult populations. A deterministic model was used to assess the chronic and acute exposures based on the Joint Meeting on Pesticide Residues （JMPR） method. A potential acute risk was demonstrated for children in the case of bifenthrin, which was found to be present at 105.36% of the acute reference dose （ARfD） value. The long- term exposure of the Chinese consumer to pesticide residues through the consumption of raw pears was far below the acceptable daily intake （ADI） criterion. Additionally, the matrix ranking scheme was used to classify risk subgroups of pesticides and pear samples. In general, 95.5% of samples were deemed to be safe and nine pesticides were classified as being of a relatively high risk. The findings indicated that the occurrence of pesticide residues in pears should not be considered a serious public health problem. Nevertheless, a more detailed study is required for vulnerable consumer groups, especially children. Continuous monitoring of pesticides in pears and tighter regulation of pesticide residue standards are recommended.展开更多
This paper reviewed management of pesticide residues in China including laws and regulations, the supervision system, the standard system, and the quality and safety of agricultural products. The process of establishm...This paper reviewed management of pesticide residues in China including laws and regulations, the supervision system, the standard system, and the quality and safety of agricultural products. The process of establishment and internationalization of standards for pesticide residues were also discussed. Results indicate that the progress of the management of pesticide residues has been steadily made in China. However, the following aspects which refer to updates to regulations, supervising efficiency, standard system, risk assessment, international cooperation and communication, should be further improved. China should draw lessons from international experience, and then establish its own management system, which focuses on pesticides controls by strictly following relevant laws and technical standards to ensure the quality and safety of agricultural products.展开更多
To improve pesticide residues detection efficiency in tea, simultaneous de- termination of eight pesticide residues in green tea was developed based on gas chromatography-mass spectrometry （GC-MS）. The results showe...To improve pesticide residues detection efficiency in tea, simultaneous de- termination of eight pesticide residues in green tea was developed based on gas chromatography-mass spectrometry （GC-MS）. The results showed that, - detected by the GC-MS under following conditions： acetonitrile as extraction and elution solvent, activated carbon and PSA tandem column as the stationary phase, elution volume of 12 ml the relationship between peak area and concentration of each residue （ametryn in the range of 0-100 pg/L, napropamide in the range of 0-10 000 gg/L, other pesticides in the range of 0-1 000 tJg/L） were linearly related, and their corre- lation coefficients were all greater than 0.999. The recovery rate the pesticides added to tea sample at legal concentration limits ranged from 73.6% to 116.8%, and the relative standard deviation from 1.47% to 15.58%. The new method we de- veloped is sensitive, specific and anti-interference, and thus provides test basis for the development of pesticide matrix reference materials in tea.展开更多
A novel thermal biosensor based on enzyme reaction for pesticides detection has been developed. This biosensor is a flow injection analysis system and consists of two channels with enzyme reaction column and identical...A novel thermal biosensor based on enzyme reaction for pesticides detection has been developed. This biosensor is a flow injection analysis system and consists of two channels with enzyme reaction column and identical reference column, which is set for eliminating the unspecific heat. The enzyme reaction takes place in the enzyme reaction column at a constant temperature(40℃) realized by a thermoelectric thermostat. Thermosensor based on the thermoelectric module containing 127 serial BiTe-thermocouples is used to monitor the temperature difference between two effluents from enzyme reaction column and reference column. The ability of this biosensor to detect pesticides is demonstrated by the decreased degree of the hydrolytic heat in two types of thermosensor mode. The hydrolytic reaction is inhibited by 36% at 1 mg/L DDVP and 50 % at 10 mg/L DDVP when cell-typed thermosensor is used. The percent inhibition is 30% at 1 mg/L DDVP and 42% at 10 mg/L DDVP in tube-typed thermosensor mode. The detection for real sample shows that this biosensor can be used for detection of organophosphate pesticides residue.展开更多
Plant pesticide residues, such as chinaberry （Melia toosendan） residue and sand cypress （Sabina vulgaris） residue, are pesticidal plant materials discarded after the bioactive ingredient has been extracted with or...Plant pesticide residues, such as chinaberry （Melia toosendan） residue and sand cypress （Sabina vulgaris） residue, are pesticidal plant materials discarded after the bioactive ingredient has been extracted with organic solvents. The only option for botanical pesticide residue utilization has been as landfill. Chinaberry residue （CBR） and sand cypress residue （SCR） were collected and composted in Yangling, Shaanxi Province, China. We studied the effects of chinaberry residue compost （CBRC）, CBRC incorporated with Trichoderma viride （CBRCT）, sand cypress residue compost （SCRC）, and SCRC incorporated with T. viride （SCRCv） on the root-knot nematode, Meloidogyne incognita, infesting the balloonflower （Platycodon grandiflorum）. Bioassay results indicated that stock solutions of the CBRCT and SCRCT extracts significantly inhibited egg hatching and caused high larval mortality, followed in degree by the CBRC and SCRC extracts. The CBR and SCR extracts caused very low inhibition of eggs and larvae. Supplementing potting mixtures with these four composts reduced the severity of root galling and increased the proportion of marketable roots. The severity of root galling decreased and the average weight of the marketable roots increased with an increase in all the composts when supplemented at rates from 5 to 30%. CBR- and SCR-supplemented pot soils also inhibited the nematodes, but CBR and SCR applied to the soil had a phytotoxic effect and inhibited balloonflower growth. Supplementing field soil with the composts reduced the severity of root galling and the populations of southern root-knot nematodes in the soil. CBRCT and SCRCT clearly enhanced the average weight of the marketable roots by 30.45 and 26.64%, respectively. Continuous supplementation with CBRCT or SCRCT in the same field significantly enhanced the control of the root-knot nematode, and the populations of nematodes continued to decrease with second inoculations. The populations of total Trichoderma spp. were distinctly enhanced and were maintained at high levels for a long time in the supplemented soils.展开更多
This study established a method for the simultaneous determination of 74 pesticide residues in Panax notoginseng by QuEChERS pretreatment method coupled with GC-MS/MS,and carried out pesticide residue analysis on 20 b...This study established a method for the simultaneous determination of 74 pesticide residues in Panax notoginseng by QuEChERS pretreatment method coupled with GC-MS/MS,and carried out pesticide residue analysis on 20 batches of market samples in China.The samples were extracted with acetonitrile,cleaned up with primary secondary amine(PSA)and octadecylsilane(C18)and determined by GC-MS/MS in multiple reaction monitoring(MRM)mode.Matrix-matched calibration was recommended to combat the matrix effect.A good linearity was observed in the range of 10−500 ng/mL with correlation coefficients≥0.9950.The mean recoveries for most of the pesticides were in the range of 70%−120%with RSD<20%.The limits of detection ranged 0.28–2.00μg/kg,while the limits of quantification were 0.94–6.65μg/kg.Following the application of“top-down”approach,the expanded measurement uncertainty for all the analytes was<30%.The proposed method was successfully applied to determine pesticide residues in 20 market samples in China,where 9 pesticides were detected and quintozene exceeded the criteria domestically and abroad.展开更多
A new method for screening and identification 420 pesticide residues in fruits and vegetables by ultra-performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry(UPLC-Q-TOF/MS)were deve...A new method for screening and identification 420 pesticide residues in fruits and vegetables by ultra-performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry(UPLC-Q-TOF/MS)were developed.The samples were extracted with acetonitrile/acetic acid(99:1,V/V),and clean-up by SinChERS-Nano(single-step,cheap,effective,rugged,safe,nano)column,determined by UPLC-Q-TOF/MS.The accurate mass database and MS/MS database which contains 420 pesticides were established,the automatic retrieval of detection results was carried on according to the accurate mass,retention time,isotope ratio,ion fragment information,and so on.Method verification was performed on leeks samples.The results showed that 420 pesticides had good linearity in the range of 0.1-100μg/L,and the correlation coeffificients(R2)was greater than 0.990.The limits of detections(LODs)and limits of quantifications(LOQs)of 420 pesticides were in range of 0.05-2.0 and 0.1-5.0μg/L,respectively.The average spike recoveries at 3 levels were 70.1%to 119.7%,and the relative standard deviations(RSD)were lower than 20%(n=6).With this method,a survey of pesticide residues was conducted for 110 samples of 10 different fruits and vegetables,which provided scientific data for ensuring pesticide residue safety of the fruits and vegetables consumed daily by the public.This method was simple,sensitive and accurate,and could be used for rapid screening of 420 pesticide residues in fruits and vegetables.展开更多
基金supported by the National Science Foundation of China(No.61101027)Qingdao Science and Technology Program(No.12-1-4-6-(8)-jch)+2 种基金Shangdong Provincial Young and Middle-Aged Scientists Research Awards Fund(No.BS2012DX032)Shandong Provincial Natural Science Foundation(No.ZR2013FM018)SDUST Research Funds(Nos.2011KYJQ101 and 2012KYTD103)
文摘Increasing awareness concerning food safety problems has been driving the search for simple and efficient biochemical analytical methods.In this paper,we develop a portable electro-acoustic biosensor based on a film bulk acoustic resonator for the detection of pesticide residues in agricultural products.A shear mode ZnO film bulk acoustic resonator with a micro-machining structure was fabricated as a mass-sensitive transducer for the real-time detection of antibody-antigen reactions in liquids.In order to obtain an ultra-low detection level,the artificial antigens were immobilized on the sensing surface of the resonator to employ a competitive format for the immunoassays.The competitive immunoreactions can be observed clearly through monitoring the frequency changes.The presence of pesticides was detected through the diminution of the frequency shift compared with the level without pesticides.The limit of detection for carbaryl(a widely used pesticide for vegetables and crops)is2?10-10 M.The proposed device represents a potential alternative to the complex optical systems and electrochemical methods that are currently being used,and represents a significant opportunity in terms of simplicity of use and portability for on-site food safety testing.
基金Supported by The Fourth Batch of High-end Talent Project in Hebei ProvinceSpecial Project of the Central Government in Guidance of Local Science and Technology Development(226Z5504G)Tangshan Talent Project(A202202005)。
文摘The QuEChERS extraction technique is a pretreatment technique that has been rapidly applied in recent years and is widely used in the field of pesticide residues with many advantages. This technique is based on solid phase extraction (SPE), which uses the interaction between adsorbent and impurities in the matrix to achieve the purpose of purification. The method has easier operation and better purification effect than SPE. In this paper, the research progress of the QuEChERS technique in pesticide residue detection in different fields in recent years and its future development were reviewed, hoping to provide reference for further development and utilization of the QuEChERS technique in pesticide residue detection in the future.
基金Supported by The Fourth Batch of High-end Talent Project in Hebei Province.
文摘[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry(GC-MS)in selective ion scanning mode(SIM).[Results]The organophosphorus pesticide standard solutions showed good linearity in the mass concentration range of 0.1-10.0μg/ml with correlation coefficients(r)not lower than 0.999,and the detection limits(S=3 N)ranged from 0.01 to 0.05 mg/kg.The average recovery values were in the range of 80.2%-99.7%,with relative standard deviations(RSDs,n=3)in the range of 1.8%-6.3%,at the addition levels of 0.5,1.0 and 2.0 mg/kg.[Conclusions]The method is simple,sensitive and accurate,and can be used for the determination of organophosphorus pesticide residues in mutton.
基金the financial support provided by the National Key R&D Program of China(2022YFA1207400)the National Key R&D Program of China(2021YFD1700105)+1 种基金the National Key R&D Program of China(2021YFA0716702)the Program of Introducing Talents of Discipline to Universities of China(111 program,B17019).
文摘Pesticide residues treatment is a crucial issue for both agricultural production and environmental protection.In recent years,designing self-cleaning nanoformulations has emerged as a promising strategy for reducing pesticide residues in a convenient and cost-effective manner.However,traditional physical blending methods of photodegradation reagents with nanocarriers have limitations in terms of pesticide residue degradation efficiency and active ingredient efficacy.Here,a new type of timing self-cleaning nanoherbicide dicamba@mSiO_(2)/ATA/TiO_(2)with a triple structure was fabricated.Dicamba,a widely used herbicide that was attracting increasing concern over its high efficiency and broad spectrum,was selected as the model herbicide and loaded on the mSiO_(2)shell.In the stage of pesticide release,the TiO_(2)and dicamba were separated by the timing-barrier.Therefore,the efficacy of dicamba was not affected by the photocatalyst.During the release process,the ATA layer continuously absorbed the reactive oxygen species(ROS)produced by TiO_(2)and was gradually degraded.Finally,the barrier was destroyed,and the residual dicamba in the carrier was degraded by TiO_(2).Compared with the traditional physical blending method,this triple structure avoided the degradation of active ingredients by photocatalysts during the pesticide release period.The experimental results suggested that this nanoformulation improved the efficacy of the herbicide,and reduced the pesticide residues,providing a new approach for self-cleaning nanopesticides research.
基金Supported by Special Fund for Scientific Research on Public Welfare by China Quality Monitoring Bureau (200910181)National Natural Science Foundation of China (60902095)~~
文摘[Objective] The aim was to explore the application of terahertz （THz） technique in pesticide recognition and residue determination. [Method] THz far-infrared spectral characteristics of 2 herbicides （butachlor and metolachlor） were measured by THz time-domain spectroscopy （THz-TDS） under conditions of room temperature and nitrogen,meanwhile their refractive index and absorption coefficient between 0.2 and 2.2 THz were calculated by using models based on Fresenl equations. [Result] The 2 pesticides both had a series of different characteristic absorption peaks between 0.2 and 2.2 THz,respectively. Their molecular structures were similar,but there were great difference in absorption and refractive index spectrum between them. [Conclusion] THz-TDS technique is feasible to detect pesticide residues,especially there is a greater advantage in identifying the structure of similar substances.
基金Supported by the Special Funds for Supervision on the Quality and Safety of Agricultural Products(GJFP201601503)~~
文摘[Objective] This study was conducted to develop a system for simultaneous determination of imidacloprid, diflubenzuron, thiabendazole and carbendazim in fruit juice by HPLC. [Method] Using acetonitrile as the extraction solvent, the pesticides in fruit juice were purified through a NH2 solid phase extraction （SPE） cartridge, then detected by HPLC. [Result] There was a good linear relationship between the peak area and the concentrations of imidacloprid, diflubenzuron, thiabendazole and carbendazim in a range of 0.05-5.0 μg/ml, and the linear correlation coefficient varied in a range of 0.999 0-0.999 8; the limit of detection for imidacloprid, diflubenzuron, thiabendazole and carbendazim was 0.003, 0.005, 0.003 and 0.007 mg/kg, respectively. The recovery rate of imidacloprid, diflubenzuron, thiabendazole and carbendazim standards added at three levels （0.1, 0.5 and 1.0 mg/kg） ranged from 82% to 107%, with RSD less than 4.5%. [Conclusion] The sensitivity, accuracy and precision of this method were able to meet the requirements for pesticide residue analysis.
文摘[Objective] A method was developed for the determination of 10 pyrethroids pesticide residues in rice by GC-MS-MS. [Method] Pyrethroids were extracted with acetonitrile, followed by a salting-out step with anhydrous magnesium sulfate and sodium chloride, cleaned up by florisil solid phase extraction （SPE） cartridge, and determined by multiple reaction monitoring mode. [Result] The method showed good linearity over the range of 0.010-0.500 mg/L for 10 pyrethroid pesticide with correlation coefficients over 0.99. The detection limits were 0.005 -0.010 mg/kg. The method was validated by analyzing samples spiked with 0.05, 0.10, 0.20 mg/kg of 10 pyrethroid pesticides, respectively. The average recoveries in rice ranged from 75.0-115.5%, and the relative standard deviations （RSD） were between 3.9%-6.9%. [Conclusion] The method is easy, accurate and reliable, which can meet the requirement for the simultaneous determination and confirmation of pyrethroid pesticide residues in rice.
基金Supported by Special Funds of National Agricultural product Quality and Safety Risk Assessment(GJFP201600402)Youth Foundation of Hubei Academy of Agricultural Sciences(2015NKYJJ36)~~
文摘The analysis of pesticide residues in Citrus from Yichang, Danjiangkou, Zigui and Xingshan in Hubei Province was accomplished by UPLC-MS and GC-MS. The results showed that the detection rate of pesticide residues in Citrus reticulate was 91.9%. The detection rate of banned pesticides was 1.6%. The detection rate of restricted pesticides was 9.5%. The detection rate of allowed pesticides was 68.3%. The detection rate of unregistered pesticides was 15.9%. The pesticide used in citrus was relatively common. Because of the banned and restricted pesticides were both in the control degree, on the whole, the quality and security of Citrus reticulata was safe.
基金Supported by the Technology System Project of National Vegetable Industry(CARS-25-A-13)Science and Technology Planning Project of Tianjin City(12ZCDZNC03600)Major Science and Technology Engineering Project of Tianjin City(12ZCDZNC03500)~~
文摘In order to study the difference between cauliflower varieties with ball well protected and unprotected in terms of pesticide residue and its causes, Jinpin 70, a new male sterile cauliflower variety with ball well protected, and Xuebao with ball unprotected were sprayed with high-toxic pesticide phorate and efficient bio-pesticide emamectin benzoate at a regular dose to investigate the impact of different cauliflower varieties on the pesticide residue. The results showed that from the 3rd to the 5th day after spraying, phorate and emamectin benzoate residues in Jinpin 70 with ball well protected reduced by 76.47%-87.65% and 67.86%-80.82% re- spectively compared with Xubao, and decreased by 9.23%-81.82% and 57.14%- 79.84% respectively compared with Jinpin 70 with ball unprotected. The results above demonstrates that inner leaves of cauliflower with ball well protected can prevent the ball from being polluted by phorate and emamectin benzoate, thereby improving its edible safety.
文摘The pretreatment and analytical techniques for organochiorine residues, including ultrasonic extraction, accelerated solvent extraction pesticide microwave extraction, solid phase extraction, and solid-phase micro-extraction and the analytical techniques of gas chromatography and gas chromatography-mass spectrometry）in tea samples in recent years were reviewed. The prospect of organochlorine pesti- cide residue analysis was proposed in this paper.
基金The Youth Foundation of the Department of Education of Hebei Province in 2016(QN2016243)
文摘This study was aimed to do the prediction of pesticide residues based on fuzzy system. Taking chlorpyrifos as an example, the Mathematic Fuzzy System was established by using the MRL values （maximum residue limits of all kinds of pesticides in food） of the Matlab Fuzzy Toolbox to analyze and predict the degra- dation degree of pesticide residues of the same crop at different time periods of bagging treatment, with the aim to provide some theoretical guidances for solving practical problems in real life.
基金Project supported by the Outstanding Young Scholar Fund and Innovative Research Group of the National Natural Science Foundation of China (No. 40325001, 40621001)the National Basic Research and Development Program of China (No. 2002CB410805) the Natural Science Foundation of Jiangsu Province (No. BK2005220).
文摘A field study was conducted in the Taihu Lake region, China in 2004 to reveal the organochlorine pesticide concentrations in soils after the ban of these substances in the year 1983. Thirteen organochlorine pesticides （OCPs） were analyzed in soils from paddy field, tree land and fallow land. Total organochlorine pesticide residues were higher in agricultural soils than in uncultivated fallow land soils. Among all the pesticides, ΣDDX （DDD, DDE and DDT） had the highest concentration for all the soil samples, ranging from 3.10 ng/g to 166.55 ng/g with a mean value of 57.04 ng/g and followed by ΣHCH, ranging from 0.73 ng/g to 60.97 ng/g with a mean value of 24.06 ng/g. Dieldrin, endrin, HCB and α-endosulfan were also found in soils with less than 15 ng/g. Ratios of p,p＇-（DDD＋DDE）/DDT in soils under three land usages were： paddy field 〉 tree land 〉 fallow land, indicating that land usage inlfuenced the degradation of DDT in soils. Ratios of p,p＇-（DDD＋DDE）/DDT 〉1, showing aged residues of DDTs in soils of the Taihu Lake region. The results were discussed with data from a former study that showed very low actual concentrations of HCH and DDT in soils in the Taihu Lake region, but according to the chemical half-lives and their concentrations in soils in 1980s, the concentration of DDT in soils seemed to be underestimated. In any case our data show that the ban on the use of HCH and DDT resulted in a tremendous reduction of these pesticide residues in soils, but there are still high amounts of pesticide residues in soils, which need more remediation processes.
文摘To ensure the safety of the commercially available chenpi,a convenient and fast analytical method was developed for the determination of 133 pesticide residues in chenpi using gas chromatography-tandem mass spectrometry(GC-MS/MS).In this study,different extraction solvents,redissolution solvents and adsorbents were tested according to the recovery and purification effect to obtain a modified QuEChERS method.The samples were extracted with acetonitrile.During the clean-up step,octadecyl-modified silica(C18)and graphitized carbon black(GCB)were selected,and aminopropyl(NH2)was used instead of primary secondary amine(PSA)because of its weaker ion exchange capacity which had little effect on the recovery of ditalimfos.Samples were quantified by matrix-matched calibration with internal standards.All pesticides showed good linearity in the respective range,both with values of r2>0.99.The average recoveries of the pesticides spiked samples ranged from 70.0% to 112.2% with the RSDs of 0.2%–14.4%.The modified QuEChERS method was validated and applied to twenty real samples.Five pesticides were found in eight batches,but no pesticide exceeded the maximum residue limits(MRL,MRL reference to European commission).
基金financially supported by the National Program for Quality and Safety Risk Assessment of Agricultural Products of China (GJFP2014002, GJFP2015002)the Core Research Budget of the Non-Profit Governmental Research Institution of China (0032014013)
文摘The presence of pesticide residues in pears is a serious health concern. This study presents the results from a 2-year investigation （2013-2014） that used gas chromatography, GS/MS and UPLC/MS-MS to measure the levels of 104 pesti- cides in 310 pear samples. In 93.2% of the samples, 43 pesticides were detected, of which the maximum residue levels （MRLs） were exceeded in 2.6% of the samples. Multiple residues （two to eight compounds） were present in 69.7% of the samples; one sample contained nine pesticides and one sample contained 10. Only 6.8% of the samples did not contain residues. To assess the health risks, the pesticide residue data have been combined with daily pear consumption data for children and adult populations. A deterministic model was used to assess the chronic and acute exposures based on the Joint Meeting on Pesticide Residues （JMPR） method. A potential acute risk was demonstrated for children in the case of bifenthrin, which was found to be present at 105.36% of the acute reference dose （ARfD） value. The long- term exposure of the Chinese consumer to pesticide residues through the consumption of raw pears was far below the acceptable daily intake （ADI） criterion. Additionally, the matrix ranking scheme was used to classify risk subgroups of pesticides and pear samples. In general, 95.5% of samples were deemed to be safe and nine pesticides were classified as being of a relatively high risk. The findings indicated that the occurrence of pesticide residues in pears should not be considered a serious public health problem. Nevertheless, a more detailed study is required for vulnerable consumer groups, especially children. Continuous monitoring of pesticides in pears and tighter regulation of pesticide residue standards are recommended.
基金supported by the National Natural Science Foundation of China (31371970)
文摘This paper reviewed management of pesticide residues in China including laws and regulations, the supervision system, the standard system, and the quality and safety of agricultural products. The process of establishment and internationalization of standards for pesticide residues were also discussed. Results indicate that the progress of the management of pesticide residues has been steadily made in China. However, the following aspects which refer to updates to regulations, supervising efficiency, standard system, risk assessment, international cooperation and communication, should be further improved. China should draw lessons from international experience, and then establish its own management system, which focuses on pesticides controls by strictly following relevant laws and technical standards to ensure the quality and safety of agricultural products.
基金Supported by Science and Technology Program of Fujian Province-Development and Application of Matrix Reference Materials of Harmful Residues in Food(2012Y6001)Development of Matrix Reference Materials of Multi-pesticide Residues in Tea based on Drug Metabolism(2012J01060)~~
文摘To improve pesticide residues detection efficiency in tea, simultaneous de- termination of eight pesticide residues in green tea was developed based on gas chromatography-mass spectrometry （GC-MS）. The results showed that, - detected by the GC-MS under following conditions： acetonitrile as extraction and elution solvent, activated carbon and PSA tandem column as the stationary phase, elution volume of 12 ml the relationship between peak area and concentration of each residue （ametryn in the range of 0-100 pg/L, napropamide in the range of 0-10 000 gg/L, other pesticides in the range of 0-1 000 tJg/L） were linearly related, and their corre- lation coefficients were all greater than 0.999. The recovery rate the pesticides added to tea sample at legal concentration limits ranged from 73.6% to 116.8%, and the relative standard deviation from 1.47% to 15.58%. The new method we de- veloped is sensitive, specific and anti-interference, and thus provides test basis for the development of pesticide matrix reference materials in tea.
文摘A novel thermal biosensor based on enzyme reaction for pesticides detection has been developed. This biosensor is a flow injection analysis system and consists of two channels with enzyme reaction column and identical reference column, which is set for eliminating the unspecific heat. The enzyme reaction takes place in the enzyme reaction column at a constant temperature(40℃) realized by a thermoelectric thermostat. Thermosensor based on the thermoelectric module containing 127 serial BiTe-thermocouples is used to monitor the temperature difference between two effluents from enzyme reaction column and reference column. The ability of this biosensor to detect pesticides is demonstrated by the decreased degree of the hydrolytic heat in two types of thermosensor mode. The hydrolytic reaction is inhibited by 36% at 1 mg/L DDVP and 50 % at 10 mg/L DDVP when cell-typed thermosensor is used. The percent inhibition is 30% at 1 mg/L DDVP and 42% at 10 mg/L DDVP in tube-typed thermosensor mode. The detection for real sample shows that this biosensor can be used for detection of organophosphate pesticides residue.
基金supported by the Important Projec of China's Western Development (2004BA901A14)
文摘Plant pesticide residues, such as chinaberry （Melia toosendan） residue and sand cypress （Sabina vulgaris） residue, are pesticidal plant materials discarded after the bioactive ingredient has been extracted with organic solvents. The only option for botanical pesticide residue utilization has been as landfill. Chinaberry residue （CBR） and sand cypress residue （SCR） were collected and composted in Yangling, Shaanxi Province, China. We studied the effects of chinaberry residue compost （CBRC）, CBRC incorporated with Trichoderma viride （CBRCT）, sand cypress residue compost （SCRC）, and SCRC incorporated with T. viride （SCRCv） on the root-knot nematode, Meloidogyne incognita, infesting the balloonflower （Platycodon grandiflorum）. Bioassay results indicated that stock solutions of the CBRCT and SCRCT extracts significantly inhibited egg hatching and caused high larval mortality, followed in degree by the CBRC and SCRC extracts. The CBR and SCR extracts caused very low inhibition of eggs and larvae. Supplementing potting mixtures with these four composts reduced the severity of root galling and increased the proportion of marketable roots. The severity of root galling decreased and the average weight of the marketable roots increased with an increase in all the composts when supplemented at rates from 5 to 30%. CBR- and SCR-supplemented pot soils also inhibited the nematodes, but CBR and SCR applied to the soil had a phytotoxic effect and inhibited balloonflower growth. Supplementing field soil with the composts reduced the severity of root galling and the populations of southern root-knot nematodes in the soil. CBRCT and SCRCT clearly enhanced the average weight of the marketable roots by 30.45 and 26.64%, respectively. Continuous supplementation with CBRCT or SCRCT in the same field significantly enhanced the control of the root-knot nematode, and the populations of nematodes continued to decrease with second inoculations. The populations of total Trichoderma spp. were distinctly enhanced and were maintained at high levels for a long time in the supplemented soils.
基金the National Key Research and Development Plan of China(2017YFC1702500).
文摘This study established a method for the simultaneous determination of 74 pesticide residues in Panax notoginseng by QuEChERS pretreatment method coupled with GC-MS/MS,and carried out pesticide residue analysis on 20 batches of market samples in China.The samples were extracted with acetonitrile,cleaned up with primary secondary amine(PSA)and octadecylsilane(C18)and determined by GC-MS/MS in multiple reaction monitoring(MRM)mode.Matrix-matched calibration was recommended to combat the matrix effect.A good linearity was observed in the range of 10−500 ng/mL with correlation coefficients≥0.9950.The mean recoveries for most of the pesticides were in the range of 70%−120%with RSD<20%.The limits of detection ranged 0.28–2.00μg/kg,while the limits of quantification were 0.94–6.65μg/kg.Following the application of“top-down”approach,the expanded measurement uncertainty for all the analytes was<30%.The proposed method was successfully applied to determine pesticide residues in 20 market samples in China,where 9 pesticides were detected and quintozene exceeded the criteria domestically and abroad.
基金supported by National Key Research and Development Program of China(2018YFC1603400)Special Technical Support Project of State Administration for Market Regulation(2019YJ009).
文摘A new method for screening and identification 420 pesticide residues in fruits and vegetables by ultra-performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry(UPLC-Q-TOF/MS)were developed.The samples were extracted with acetonitrile/acetic acid(99:1,V/V),and clean-up by SinChERS-Nano(single-step,cheap,effective,rugged,safe,nano)column,determined by UPLC-Q-TOF/MS.The accurate mass database and MS/MS database which contains 420 pesticides were established,the automatic retrieval of detection results was carried on according to the accurate mass,retention time,isotope ratio,ion fragment information,and so on.Method verification was performed on leeks samples.The results showed that 420 pesticides had good linearity in the range of 0.1-100μg/L,and the correlation coeffificients(R2)was greater than 0.990.The limits of detections(LODs)and limits of quantifications(LOQs)of 420 pesticides were in range of 0.05-2.0 and 0.1-5.0μg/L,respectively.The average spike recoveries at 3 levels were 70.1%to 119.7%,and the relative standard deviations(RSD)were lower than 20%(n=6).With this method,a survey of pesticide residues was conducted for 110 samples of 10 different fruits and vegetables,which provided scientific data for ensuring pesticide residue safety of the fruits and vegetables consumed daily by the public.This method was simple,sensitive and accurate,and could be used for rapid screening of 420 pesticide residues in fruits and vegetables.
