建立血液中呋喃芬太尼的LC-QTOF-MS检验方法。采用Eclipse Plus C18(1.8μm,3.0X150mm)色谱柱,以水相A(0.1%(v/v)甲酸和5mM乙酸铵的水溶液)和有机相B(乙腈)为流动相梯度洗脱,质谱采用电喷雾正离子全扫描模式,对血液中的呋喃芬太尼分析...建立血液中呋喃芬太尼的LC-QTOF-MS检验方法。采用Eclipse Plus C18(1.8μm,3.0X150mm)色谱柱,以水相A(0.1%(v/v)甲酸和5mM乙酸铵的水溶液)和有机相B(乙腈)为流动相梯度洗脱,质谱采用电喷雾正离子全扫描模式,对血液中的呋喃芬太尼分析检验。方法回收率为76.44%~92%,线性回归方程为y=4355.5 x+2242.9,检出限为0.1 ng·mL^(-1),定量限为2 ng·mL^(-1)。本方法操作简单,可为定性定量分析检测血液中的呋喃芬太尼提供数据帮助。展开更多
OBJECTIVE Identification of pesticide residues in TCM herbs is important for drug safety and public health.However,it is very challenging for the development of an instrument-based multi-residue pesticide analysis met...OBJECTIVE Identification of pesticide residues in TCM herbs is important for drug safety and public health.However,it is very challenging for the development of an instrument-based multi-residue pesticide analysis method for theherbalproducts due to their complex matrix.This study aims to develop a rapid method for the high-throughput detection of pesticide residues in TCM herbal products using liquid chromatography coupled to quadrupoletime of flight(LC-QTOF)mass spectrometry.METHODS In this study,we attempt to investigate possible pesticide residues in TCM herbal products which are commonly available in Singapore and to consolidate a comprehensive pesticide database for more than 250 regulated pesticides in FDA Regulations.We also attempt to perform non-targeted and targeted screenings of pesticide residues in herbal products by searching our database.RESULTS The developed LC-QTOF method demonstrates have high mass accuracy,resolution and selectivity,which makes it a very suitable tool for monitoring both target and non-target pesticides with a limit of detection at the low ppb level.Moreover,the LC-QTOF technology permits to retain all spectral data in a single run.It may avoid many difficulties related to matrix effects and will save much manpower.CONCLUSIONThis means that a variety of TCM herbs can be easily detected by this method for the presence or absence of pesticide residues that must conform to government regulations.展开更多
基于液相色谱-四极杆/飞行时间质谱(LC-QTOF-MS)建立了药物中27种新型毒品芬太尼类物质(芬太尼及其类似物)的同时快速筛查、确证和定量分析方法。样品经5 mL 75%(v/v)乙腈水溶液和5 mL乙腈提取,HLB固相萃取柱净化,电喷雾电离,正离子扫描...基于液相色谱-四极杆/飞行时间质谱(LC-QTOF-MS)建立了药物中27种新型毒品芬太尼类物质(芬太尼及其类似物)的同时快速筛查、确证和定量分析方法。样品经5 mL 75%(v/v)乙腈水溶液和5 mL乙腈提取,HLB固相萃取柱净化,电喷雾电离,正离子扫描,TOF-MS和信息依赖性采集(IDA)-MS/MS采集模式检测,外标法定量;建立一级精确质量数据库、保留时间和二级质谱库,实现了固体压片、粉末、液体药物及透皮贴剂中27种芬太尼类物质的快速筛查和确证。在5.00~100μg/L范围内,27种目标化合物的线性关系良好(r2>0.99)。27种化合物的定量限均为10.0μg/kg。在维生素C压片、头痛粉、止咳水、透皮贴剂样品中3个添加水平的平均回收率范围分别82.9%~106%、84.8%~106%、86.9%~109%和83.1%~106%,相对标准偏差(RSD)为0.38%~8.71%(n=6)。本方法操作简便,耗时短,灵敏度高,稳定性好,适用于液体和固体药物中芬太尼类物质的筛查检测及定量分析,可显著降低检测成本,具有实际应用价值。展开更多
文摘OBJECTIVE Identification of pesticide residues in TCM herbs is important for drug safety and public health.However,it is very challenging for the development of an instrument-based multi-residue pesticide analysis method for theherbalproducts due to their complex matrix.This study aims to develop a rapid method for the high-throughput detection of pesticide residues in TCM herbal products using liquid chromatography coupled to quadrupoletime of flight(LC-QTOF)mass spectrometry.METHODS In this study,we attempt to investigate possible pesticide residues in TCM herbal products which are commonly available in Singapore and to consolidate a comprehensive pesticide database for more than 250 regulated pesticides in FDA Regulations.We also attempt to perform non-targeted and targeted screenings of pesticide residues in herbal products by searching our database.RESULTS The developed LC-QTOF method demonstrates have high mass accuracy,resolution and selectivity,which makes it a very suitable tool for monitoring both target and non-target pesticides with a limit of detection at the low ppb level.Moreover,the LC-QTOF technology permits to retain all spectral data in a single run.It may avoid many difficulties related to matrix effects and will save much manpower.CONCLUSIONThis means that a variety of TCM herbs can be easily detected by this method for the presence or absence of pesticide residues that must conform to government regulations.
文摘基于液相色谱-四极杆/飞行时间质谱(LC-QTOF-MS)建立了药物中27种新型毒品芬太尼类物质(芬太尼及其类似物)的同时快速筛查、确证和定量分析方法。样品经5 mL 75%(v/v)乙腈水溶液和5 mL乙腈提取,HLB固相萃取柱净化,电喷雾电离,正离子扫描,TOF-MS和信息依赖性采集(IDA)-MS/MS采集模式检测,外标法定量;建立一级精确质量数据库、保留时间和二级质谱库,实现了固体压片、粉末、液体药物及透皮贴剂中27种芬太尼类物质的快速筛查和确证。在5.00~100μg/L范围内,27种目标化合物的线性关系良好(r2>0.99)。27种化合物的定量限均为10.0μg/kg。在维生素C压片、头痛粉、止咳水、透皮贴剂样品中3个添加水平的平均回收率范围分别82.9%~106%、84.8%~106%、86.9%~109%和83.1%~106%,相对标准偏差(RSD)为0.38%~8.71%(n=6)。本方法操作简便,耗时短,灵敏度高,稳定性好,适用于液体和固体药物中芬太尼类物质的筛查检测及定量分析,可显著降低检测成本,具有实际应用价值。
