Gelsemium elegans Benth alkaloids are the main components of G.elegans and can cause acute toxicosis or even death.Although several studies have reported methods for detecting G.elegans alkaloids,a high-throughput and...Gelsemium elegans Benth alkaloids are the main components of G.elegans and can cause acute toxicosis or even death.Although several studies have reported methods for detecting G.elegans alkaloids,a high-throughput and environmental-friendly strategy for detection of multiple G.elegans alkaloids has not been realized.In this work,a matrix-assisted laser desorption/ionization time-of-flight mass spectrometry method was developed for rapid detection of G.elegans alkaloids in human plasma and urine for diagnosis of poisoning.Multiple matrices and crys-tal spotting methods were evaluated to obtain stable and high peak intensities without“sweet spot”.We verified the methodology and obtained excellent results.The matrix effects with different dilutions were compared and good recoveries and a low relative standard deviation were obtained with a 40-fold dilution.This method could shorten the analysis time and greatly reduce the consumption of chemical solvents.Furthermore,it could be applied to quan-titative assessment of G.elegans alkaloid poisoning incidents.展开更多
Objective: To develop a powerful integrated strategy based on liquid chromatography coupled with mass spectrometry(LC-MS) systems for the comprehensive characterization and quantification of multiple components of her...Objective: To develop a powerful integrated strategy based on liquid chromatography coupled with mass spectrometry(LC-MS) systems for the comprehensive characterization and quantification of multiple components of herbal medicines.Methods: Firstly, different mobile phase additives, analysis time, and MS acquisition modes were orthogonally tested with liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(LC-QTOF/MS) in order to detect as many components of Gelsemium elegans as possible with high peak intensity. Secondly, several data mining strategies, including database searching, diagnostic ion filtering and neutral loss filtering, were utilized to perform chemical profiling. Subsequently, this study focused on the quantification and validation of the performance of a liquid chromatography-triple mass spectrometry(LC-Qq Q/MS) assay based on derivative multiple reaction monitoring(De MRM).Results: A total of 147 components from G. elegans were characterized, among them 116 nontarget components were reported for the first time. A sensitive and reproducible LC-Qq Q/MS method was successfully developed and validated for the simultaneous relative quantification of 41 components of G. elegans.This LC-Qq Q/MS method was then applied to compare the contents of components in the roots, stems and leaves.Conclusion: The present integrated strategy would significantly contribute to chemical studies on herbal medicine, and its utility could be extended to other research fields, such as metabolomics, quality control,and pharmacokinetics.展开更多
基金supported by the National Natural Science Foundation of China(Grant No.32372448)Guangdong Basic and Applied Basic Research Foundation,China(Grant No.2023A1515012605)+2 种基金the Science and Technology Program of Guangdong Administration for Market Regulation,China(Grant No.2023CS01)the Science and Technology Program of National General Customs Administration of China(Grant No.2022HK108)the Science and Technology Program of Shantou City,China(Grant No.STKJ2023024).
文摘Gelsemium elegans Benth alkaloids are the main components of G.elegans and can cause acute toxicosis or even death.Although several studies have reported methods for detecting G.elegans alkaloids,a high-throughput and environmental-friendly strategy for detection of multiple G.elegans alkaloids has not been realized.In this work,a matrix-assisted laser desorption/ionization time-of-flight mass spectrometry method was developed for rapid detection of G.elegans alkaloids in human plasma and urine for diagnosis of poisoning.Multiple matrices and crys-tal spotting methods were evaluated to obtain stable and high peak intensities without“sweet spot”.We verified the methodology and obtained excellent results.The matrix effects with different dilutions were compared and good recoveries and a low relative standard deviation were obtained with a 40-fold dilution.This method could shorten the analysis time and greatly reduce the consumption of chemical solvents.Furthermore,it could be applied to quan-titative assessment of G.elegans alkaloid poisoning incidents.
基金supported by National Key R&D Program of Intergovernmental Key Projects (Grant No: 2018YFE0101700)National Natural Science Foundation of China (Grant No. 31972737)。
文摘Objective: To develop a powerful integrated strategy based on liquid chromatography coupled with mass spectrometry(LC-MS) systems for the comprehensive characterization and quantification of multiple components of herbal medicines.Methods: Firstly, different mobile phase additives, analysis time, and MS acquisition modes were orthogonally tested with liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(LC-QTOF/MS) in order to detect as many components of Gelsemium elegans as possible with high peak intensity. Secondly, several data mining strategies, including database searching, diagnostic ion filtering and neutral loss filtering, were utilized to perform chemical profiling. Subsequently, this study focused on the quantification and validation of the performance of a liquid chromatography-triple mass spectrometry(LC-Qq Q/MS) assay based on derivative multiple reaction monitoring(De MRM).Results: A total of 147 components from G. elegans were characterized, among them 116 nontarget components were reported for the first time. A sensitive and reproducible LC-Qq Q/MS method was successfully developed and validated for the simultaneous relative quantification of 41 components of G. elegans.This LC-Qq Q/MS method was then applied to compare the contents of components in the roots, stems and leaves.Conclusion: The present integrated strategy would significantly contribute to chemical studies on herbal medicine, and its utility could be extended to other research fields, such as metabolomics, quality control,and pharmacokinetics.