The purpose of the study was to establish an analytical method to simultaneously determine multiple sterols in tobacco leaves rapidly and accurately.In this gas chromatography-triple quadruple tandem mass spectrometry...The purpose of the study was to establish an analytical method to simultaneously determine multiple sterols in tobacco leaves rapidly and accurately.In this gas chromatography-triple quadruple tandem mass spectrometry(GC-MS/MS)based method,various conditions for sterols extraction were assessed and the instrumental operation parameters were optimized with 5α-cholane as an internal standard.Using this method,eight plant sterols,namely lanosterol,campesterol,chenodeoxycholic acid,cholesterol,β-sitosterol,stigmasterol,dihydrotachysterol and ergosterol,were separated in less than 30 min.The linear correlation coefficients were over 0.998 9,the low detection limits were in the range of 0.010 3-0.141 4 μg/g.The recoveries were from 87.30% to 115.60%,with low standard deviations.In conclusion,this method demonstrates good repeatability,accuracy,and high sensitivity,and is best suited for rapid analysis of multiple sterols in tobacco leaves.展开更多
A new method was developed for the simultaneous analysis of 12 pesticide residues in onion and fennel by gas chromatography(GC)-triple quadrupole mass spectrometry(MS/MS)-electron impact ion source(EI)-select reaction...A new method was developed for the simultaneous analysis of 12 pesticide residues in onion and fennel by gas chromatography(GC)-triple quadrupole mass spectrometry(MS/MS)-electron impact ion source(EI)-select reaction monitoring mode(SRM).The 12 pesticide includes fungicide,acaricide,carbamate and plant growth regulator pesticide.The complicated matrix samples of onion and fennel were extracted by acetonitrile,cleaned up by solid phase extraction of Carb/PSA.By optimizing the GC-MS/MS-SRM parameters,the interference from clean-up procedure was further removed and 12 pesticide residues were determined accurately.The average recoveries for most pesticides(at the spiked level of 0.05-0.20 mg/kg) were between 114%-156%,the relative standard deviation(RSD) of the method was less than 20%,and the limit of detection were 0.5-5 μg/kg.展开更多
为了比较不同萃取方法对茯砖茶挥发性成分的萃取效果,找到更适合茯砖茶挥发性成分分析的萃取方法,采用气相色谱-三重四极杆串联质谱(Gas Chromatography-triple Quadrupole Series Mass Spectrometry,GC-QQQ-MS)比较分析了同时蒸馏萃取...为了比较不同萃取方法对茯砖茶挥发性成分的萃取效果,找到更适合茯砖茶挥发性成分分析的萃取方法,采用气相色谱-三重四极杆串联质谱(Gas Chromatography-triple Quadrupole Series Mass Spectrometry,GC-QQQ-MS)比较分析了同时蒸馏萃取法(Simultaneous Distillation Extraction,SDE)和顶空固相微萃取法(Head Space Solid-phase Microextraction,HS-SPME)提取茯砖茶挥发性成分的效果。结果表明:两种方法提取到的茯砖茶挥发性成分差异明显,两种方法共提取出90种挥发性成分,共有成分40种。其中SDE法提取到79种,以碳氢化合物、杂氧化合物、酮类和酚类为主;主要化合物有植酮、雪松醇、棕榈酸、2,6-二叔丁基对甲酚、二苯并呋喃、菲、香叶基丙酮、邻苯二甲醚、邻甲酚、联苯等。HS-SPME法提取到50种,以碳氢化合物、杂氧化合物、酮类和酚类为主;主要化合物有咖啡因、邻苯二甲酸二乙酯、二苯并呋喃、二氢猕猴桃内酯、联苯、香叶基丙酮、植酮、雪松醇、菲、1,2,3-三甲氧基苯等。两种方法各有优劣,相互补充,结合分析可为茯砖茶挥发性成分鉴定提供更全面、更完整、更准确的信息。展开更多
文摘The purpose of the study was to establish an analytical method to simultaneously determine multiple sterols in tobacco leaves rapidly and accurately.In this gas chromatography-triple quadruple tandem mass spectrometry(GC-MS/MS)based method,various conditions for sterols extraction were assessed and the instrumental operation parameters were optimized with 5α-cholane as an internal standard.Using this method,eight plant sterols,namely lanosterol,campesterol,chenodeoxycholic acid,cholesterol,β-sitosterol,stigmasterol,dihydrotachysterol and ergosterol,were separated in less than 30 min.The linear correlation coefficients were over 0.998 9,the low detection limits were in the range of 0.010 3-0.141 4 μg/g.The recoveries were from 87.30% to 115.60%,with low standard deviations.In conclusion,this method demonstrates good repeatability,accuracy,and high sensitivity,and is best suited for rapid analysis of multiple sterols in tobacco leaves.
文摘A new method was developed for the simultaneous analysis of 12 pesticide residues in onion and fennel by gas chromatography(GC)-triple quadrupole mass spectrometry(MS/MS)-electron impact ion source(EI)-select reaction monitoring mode(SRM).The 12 pesticide includes fungicide,acaricide,carbamate and plant growth regulator pesticide.The complicated matrix samples of onion and fennel were extracted by acetonitrile,cleaned up by solid phase extraction of Carb/PSA.By optimizing the GC-MS/MS-SRM parameters,the interference from clean-up procedure was further removed and 12 pesticide residues were determined accurately.The average recoveries for most pesticides(at the spiked level of 0.05-0.20 mg/kg) were between 114%-156%,the relative standard deviation(RSD) of the method was less than 20%,and the limit of detection were 0.5-5 μg/kg.
文摘为了比较不同萃取方法对茯砖茶挥发性成分的萃取效果,找到更适合茯砖茶挥发性成分分析的萃取方法,采用气相色谱-三重四极杆串联质谱(Gas Chromatography-triple Quadrupole Series Mass Spectrometry,GC-QQQ-MS)比较分析了同时蒸馏萃取法(Simultaneous Distillation Extraction,SDE)和顶空固相微萃取法(Head Space Solid-phase Microextraction,HS-SPME)提取茯砖茶挥发性成分的效果。结果表明:两种方法提取到的茯砖茶挥发性成分差异明显,两种方法共提取出90种挥发性成分,共有成分40种。其中SDE法提取到79种,以碳氢化合物、杂氧化合物、酮类和酚类为主;主要化合物有植酮、雪松醇、棕榈酸、2,6-二叔丁基对甲酚、二苯并呋喃、菲、香叶基丙酮、邻苯二甲醚、邻甲酚、联苯等。HS-SPME法提取到50种,以碳氢化合物、杂氧化合物、酮类和酚类为主;主要化合物有咖啡因、邻苯二甲酸二乙酯、二苯并呋喃、二氢猕猴桃内酯、联苯、香叶基丙酮、植酮、雪松醇、菲、1,2,3-三甲氧基苯等。两种方法各有优劣,相互补充,结合分析可为茯砖茶挥发性成分鉴定提供更全面、更完整、更准确的信息。
