目的探究液相色谱―串联质谱仪(liquid chromatography-tandem mass spectrometer,LC-MS/MS)检测饲料中克伦普罗时,环天冬氨酰苯丙氨酸对试验干扰的原因,在此基础上探究出应用LC-MS/MS分析的确证技术与方法。方法应用四极杆―轨道阱高...目的探究液相色谱―串联质谱仪(liquid chromatography-tandem mass spectrometer,LC-MS/MS)检测饲料中克伦普罗时,环天冬氨酰苯丙氨酸对试验干扰的原因,在此基础上探究出应用LC-MS/MS分析的确证技术与方法。方法应用四极杆―轨道阱高分辨质谱仪和LC-MS/MS对环天冬氨酰苯丙氨酸、克伦普罗对照品以及含有环天冬氨酰苯丙氨酸的饲料样品进行分析。结果饲料中含有环天冬氨酰苯丙氨酸对克伦普罗的检测干扰的原因为二者母离子及2个子离子的质荷比很接近,且二者离子丰度比也很接近。应用LC-MS/MS分析的确证技术与方法为梯度碎裂离子片段依次匹配比较法。结论应用LC-MS/MS检测会遇到假阳性的问题,这是串联质谱结构与方法原理决定的;建议调整克伦普罗的2个子离子为263.07>168.04,263.07>132.06;用LC-MS的梯度碎裂离子片段依次匹配比较法准确、实用。展开更多
采用分散液液微萃取(dispersive liquid-liquid microextraction,DLLME)-超高效液相色谱-四极杆高分辨飞行时间质谱法(ultra performance liquid chromatography-high resolution quadrupole time of flight mass spectrometer,UPLC-Q-T...采用分散液液微萃取(dispersive liquid-liquid microextraction,DLLME)-超高效液相色谱-四极杆高分辨飞行时间质谱法(ultra performance liquid chromatography-high resolution quadrupole time of flight mass spectrometer,UPLC-Q-TOF-MS),对新鲜果汁中5种氨基甲酸酯类农药进行同时测定.样品先经N-丙基乙二胺(primary secondary amine,PSA)除杂,然后以甲醇为分散剂,三氯甲烷为萃取剂对目标物进行萃取.离心分层后取下层有机相分析.采用电喷雾离子源(electron spray ionization,ESI)和大气压化学电离(atmospheric pressure chemical ionization,APCI)复合源,正离子扫描方式进行数据采集.5种氨基甲酸酯类农药在2.0μg/L^200μg/L范围内呈良好线性关系,相关系数r均大于0.9990,平均回收率为84.5%~97.8%,检出限为0.02μg/kg^0.05μg/kg,定量限为0.05μg/kg^0.15μg/kg,相对标准偏差为1.28%~6.88%.展开更多
Chinese dwarf cherry(Ouli)is a native shrub in northwest China with high ecological value,but the nutritive potential remains to be explored.In this study,the total content of polyphenols,flavonoids,proanthocyanidins,...Chinese dwarf cherry(Ouli)is a native shrub in northwest China with high ecological value,but the nutritive potential remains to be explored.In this study,the total content of polyphenols,flavonoids,proanthocyanidins,and anthocyanins of Ouli from 30 germplasms were measured,and the antioxidant activities were evaluated by FRAP and ABTS assays.The polyphenol profile was determined by ultra-high-performance liquid chromatography-high resolution mass spectrometry.Grey relational analysis and partial least squares were utilized to build chemometrics models for selecting antioxidant compounds.The contents of total flavonoids,proanthocyanidins,phenols and total anthocyanidins of 30 germplasms of Ouli were 119.92-668.76 mg/100 g fresh weight(FW),90.81-555.44 mg/100 g FW,148.42-390.43 mg/100 g FW,0.02-17.26 mg/100 g FW,respectively.A total of 61 compounds were identified,including 40 flavonoids(26 flavonols,4 anthocyanins,6 dihydroflavonols,2 dihydrochalcones,and 2 flavones),12 proanthocyanidins,6 phenolic acids,and 3 types of other class compounds(one stilbene and two phenols).The proanthocyanidin compounds in Ouli contributes most to the total antioxidant capacity with the antioxidant rank that procyanidin trimer>tetramer>dimer≈monomer.Catechin and procyanidin B1 were the most abundant compounds and were 18.45-162.50μg/g FW and 30.52-149.42μg/g FW,respectively.Shanxi(SX)2 and SX10 could be considered as potential germplasms,and proanthocyanidins could be chosen as a characteristic nutrient evaluation index of Ouli.This study not only takes a key step to lay the groundwork for further research of Ouli but also provides a reference for the discovery of the functional ingredients of other foods.展开更多
文摘目的探究液相色谱―串联质谱仪(liquid chromatography-tandem mass spectrometer,LC-MS/MS)检测饲料中克伦普罗时,环天冬氨酰苯丙氨酸对试验干扰的原因,在此基础上探究出应用LC-MS/MS分析的确证技术与方法。方法应用四极杆―轨道阱高分辨质谱仪和LC-MS/MS对环天冬氨酰苯丙氨酸、克伦普罗对照品以及含有环天冬氨酰苯丙氨酸的饲料样品进行分析。结果饲料中含有环天冬氨酰苯丙氨酸对克伦普罗的检测干扰的原因为二者母离子及2个子离子的质荷比很接近,且二者离子丰度比也很接近。应用LC-MS/MS分析的确证技术与方法为梯度碎裂离子片段依次匹配比较法。结论应用LC-MS/MS检测会遇到假阳性的问题,这是串联质谱结构与方法原理决定的;建议调整克伦普罗的2个子离子为263.07>168.04,263.07>132.06;用LC-MS的梯度碎裂离子片段依次匹配比较法准确、实用。
文摘采用分散液液微萃取(dispersive liquid-liquid microextraction,DLLME)-超高效液相色谱-四极杆高分辨飞行时间质谱法(ultra performance liquid chromatography-high resolution quadrupole time of flight mass spectrometer,UPLC-Q-TOF-MS),对新鲜果汁中5种氨基甲酸酯类农药进行同时测定.样品先经N-丙基乙二胺(primary secondary amine,PSA)除杂,然后以甲醇为分散剂,三氯甲烷为萃取剂对目标物进行萃取.离心分层后取下层有机相分析.采用电喷雾离子源(electron spray ionization,ESI)和大气压化学电离(atmospheric pressure chemical ionization,APCI)复合源,正离子扫描方式进行数据采集.5种氨基甲酸酯类农药在2.0μg/L^200μg/L范围内呈良好线性关系,相关系数r均大于0.9990,平均回收率为84.5%~97.8%,检出限为0.02μg/kg^0.05μg/kg,定量限为0.05μg/kg^0.15μg/kg,相对标准偏差为1.28%~6.88%.
基金supported by the Beijing Natural Science Foundation[grant number 5212014]Key Research and Development Program in the Ningxia Hui Autonomous Region,PR China[grant number 2020BBF02027].
文摘Chinese dwarf cherry(Ouli)is a native shrub in northwest China with high ecological value,but the nutritive potential remains to be explored.In this study,the total content of polyphenols,flavonoids,proanthocyanidins,and anthocyanins of Ouli from 30 germplasms were measured,and the antioxidant activities were evaluated by FRAP and ABTS assays.The polyphenol profile was determined by ultra-high-performance liquid chromatography-high resolution mass spectrometry.Grey relational analysis and partial least squares were utilized to build chemometrics models for selecting antioxidant compounds.The contents of total flavonoids,proanthocyanidins,phenols and total anthocyanidins of 30 germplasms of Ouli were 119.92-668.76 mg/100 g fresh weight(FW),90.81-555.44 mg/100 g FW,148.42-390.43 mg/100 g FW,0.02-17.26 mg/100 g FW,respectively.A total of 61 compounds were identified,including 40 flavonoids(26 flavonols,4 anthocyanins,6 dihydroflavonols,2 dihydrochalcones,and 2 flavones),12 proanthocyanidins,6 phenolic acids,and 3 types of other class compounds(one stilbene and two phenols).The proanthocyanidin compounds in Ouli contributes most to the total antioxidant capacity with the antioxidant rank that procyanidin trimer>tetramer>dimer≈monomer.Catechin and procyanidin B1 were the most abundant compounds and were 18.45-162.50μg/g FW and 30.52-149.42μg/g FW,respectively.Shanxi(SX)2 and SX10 could be considered as potential germplasms,and proanthocyanidins could be chosen as a characteristic nutrient evaluation index of Ouli.This study not only takes a key step to lay the groundwork for further research of Ouli but also provides a reference for the discovery of the functional ingredients of other foods.
