[Objectives]This study was conducted to establish an uncertainty evaluation method for the determination of ethyl maltol by ultra-high performance liquid chromatograph-mass spectrometer(UPLC-MS).[Methods]A mathematica...[Objectives]This study was conducted to establish an uncertainty evaluation method for the determination of ethyl maltol by ultra-high performance liquid chromatograph-mass spectrometer(UPLC-MS).[Methods]A mathematical model of uncertainty was established by analyzing the method for determining ethyl maltol using UPLC-MS.The sources of uncertainty were analyzed,and the components of uncertainty were calculated to evaluate the expanded uncertainty of the method.[Results]When the content of ethyl maltol in edible vegetable oil was 1657μg/kg,the expanded uncertainty was 22.4μg/kg(K=2,P=95%).[Conclusions]The uncertainty in this evaluation model mainly came from standard solution preparation,sample weighing,dilution of sample to constant volume,standard curve fitting,and repeated measurement.展开更多
A liquid-microjet(LJ)linear time-of-flight(TOF)mass spectrometer,coupled with a femtosecond laser ionization source,has been designed for direct measurements of mass spectra of liquid aqueous solutions.Two main featur...A liquid-microjet(LJ)linear time-of-flight(TOF)mass spectrometer,coupled with a femtosecond laser ionization source,has been designed for direct measurements of mass spectra of liquid aqueous solutions.Two main features of our designed spectrometer involve the coupling of a liquid microjet nozzle to a conventional ion optics and the application of femtosecond pulses for mass spectral ionization.The detailed design,construction,and simulation of this new spectrometer are presented.More importantly,we combined the experimental tests with the simulated electric fields and ion trajectories to investigate the performance of the designed spectrometer,especially the kind of disturbances of the nozzle electric field on the conventional ion optics.In our current design,the optimal E/R(E:extractor,R:repeller)electrode voltage ratio was found to be∼0.71 when the voltages on the R,E and G(ground)electrodes were set to be 1500,1060 and 0 V,respectively,whilst the voltage on the N nozzle electrode was required to be around 1250 V.The capability of the designed spectrometer has been demonstrated by recording the simulated mass spectra of the water,benzene and cytidine with their mass/charge ratios of 18,76 and 243,respectively.This work shall be helpful for the development of new all-liquid-phase mass spectral technology to be employed in the diagnosis of diseases by the mass analysis of human body fluids.展开更多
A simultaneous method was successfully established and validated for the separation and determination of bu- prenorphine （BP）, its primary metabolite, nor-buprenorphine （NBP） and a proposed co-formulate, naloxone ...A simultaneous method was successfully established and validated for the separation and determination of bu- prenorphine （BP）, its primary metabolite, nor-buprenorphine （NBP） and a proposed co-formulate, naloxone （NLX） in human plasma. The method used buprenorphine-d4 （BP-D4）, nor-buprenorphine-d3 （NBP-D3）, naltrexone （NTX） as internal standards （ISs）. 100 μL of plasma sample fortified with the ISs was cleaned up by solid-phase extraction （SPE）, and was then separated on a Waters AcquityTM BEH C18 column with gradient elution using methanol and water （containing 0.2% formic） at a flow rate of 0.25 mL·min^-1. The mass spectrometer was used for detection and was operated in the positive electrospray ionization with multiple reaction monitoring （MRM） mode. The three compounds were effectively separated in 5 min. The linear ranges of the compounds were 0.1--25, 0.25--25 and 0.05--25 ng·mL^-1 for BP, NBP and NLX, respectively, with r≥0.9935. The method had high sensitivity （the lim- its of detection were 0.02, 0.1 and 0.01 ng.mL-1 for BP, NBP and NLX, respectively） and high recoveries （≥97.6%）. The result was shown to be linear and satisfactorily met current acceptance criteria for validation of bio- analytical method： intra and inter assay precisions within the required limits of ≤25% RSD. The LOQs fulfilled the LOQ requirements： precision≤25% RSD, and was fully validated according to the State Food and Drug Administration （SFDA） regulations. The results demonstrated that ultra-high performance liquid chromatography- tandem mass spectrometer （UPLC-MS/MS） with SPE was a powerful detection tool and contributed to pharmaceutical analysis in biological matrices.展开更多
文摘[Objectives]This study was conducted to establish an uncertainty evaluation method for the determination of ethyl maltol by ultra-high performance liquid chromatograph-mass spectrometer(UPLC-MS).[Methods]A mathematical model of uncertainty was established by analyzing the method for determining ethyl maltol using UPLC-MS.The sources of uncertainty were analyzed,and the components of uncertainty were calculated to evaluate the expanded uncertainty of the method.[Results]When the content of ethyl maltol in edible vegetable oil was 1657μg/kg,the expanded uncertainty was 22.4μg/kg(K=2,P=95%).[Conclusions]The uncertainty in this evaluation model mainly came from standard solution preparation,sample weighing,dilution of sample to constant volume,standard curve fitting,and repeated measurement.
基金supported by the Knowledge Innovation Program of Wuhan-Basic Research(Nos.2023020201010084,2022010801010134)the National Key Research and Development Program of China(No.2019YFA0307700)the National Natural Science Foundation of China(Nos.12274418,22273116,12074389,11974381,22363011).
文摘A liquid-microjet(LJ)linear time-of-flight(TOF)mass spectrometer,coupled with a femtosecond laser ionization source,has been designed for direct measurements of mass spectra of liquid aqueous solutions.Two main features of our designed spectrometer involve the coupling of a liquid microjet nozzle to a conventional ion optics and the application of femtosecond pulses for mass spectral ionization.The detailed design,construction,and simulation of this new spectrometer are presented.More importantly,we combined the experimental tests with the simulated electric fields and ion trajectories to investigate the performance of the designed spectrometer,especially the kind of disturbances of the nozzle electric field on the conventional ion optics.In our current design,the optimal E/R(E:extractor,R:repeller)electrode voltage ratio was found to be∼0.71 when the voltages on the R,E and G(ground)electrodes were set to be 1500,1060 and 0 V,respectively,whilst the voltage on the N nozzle electrode was required to be around 1250 V.The capability of the designed spectrometer has been demonstrated by recording the simulated mass spectra of the water,benzene and cytidine with their mass/charge ratios of 18,76 and 243,respectively.This work shall be helpful for the development of new all-liquid-phase mass spectral technology to be employed in the diagnosis of diseases by the mass analysis of human body fluids.
文摘A simultaneous method was successfully established and validated for the separation and determination of bu- prenorphine （BP）, its primary metabolite, nor-buprenorphine （NBP） and a proposed co-formulate, naloxone （NLX） in human plasma. The method used buprenorphine-d4 （BP-D4）, nor-buprenorphine-d3 （NBP-D3）, naltrexone （NTX） as internal standards （ISs）. 100 μL of plasma sample fortified with the ISs was cleaned up by solid-phase extraction （SPE）, and was then separated on a Waters AcquityTM BEH C18 column with gradient elution using methanol and water （containing 0.2% formic） at a flow rate of 0.25 mL·min^-1. The mass spectrometer was used for detection and was operated in the positive electrospray ionization with multiple reaction monitoring （MRM） mode. The three compounds were effectively separated in 5 min. The linear ranges of the compounds were 0.1--25, 0.25--25 and 0.05--25 ng·mL^-1 for BP, NBP and NLX, respectively, with r≥0.9935. The method had high sensitivity （the lim- its of detection were 0.02, 0.1 and 0.01 ng.mL-1 for BP, NBP and NLX, respectively） and high recoveries （≥97.6%）. The result was shown to be linear and satisfactorily met current acceptance criteria for validation of bio- analytical method： intra and inter assay precisions within the required limits of ≤25% RSD. The LOQs fulfilled the LOQ requirements： precision≤25% RSD, and was fully validated according to the State Food and Drug Administration （SFDA） regulations. The results demonstrated that ultra-high performance liquid chromatography- tandem mass spectrometer （UPLC-MS/MS） with SPE was a powerful detection tool and contributed to pharmaceutical analysis in biological matrices.
