加速溶剂萃取-气相色谱-串联质谱法测定党参中69种农药残留量
GC-MS/MS Determination of Residual Amounts of 69 Pesticides in Radix Codonopsis with Accelerate Solvent Extraction
摘 要
采用加速溶剂萃取-气相色谱-串联质谱法测定党参中69种农药残留量。样品以乙腈为溶剂经加速溶剂提取,提取液用Carb/NH2固相萃取小柱净化。在气相色谱分离中用VF-5MS柱为固定相,在质谱分析中采用多反应监测模式。69种农药在一定的质量浓度范围内与其峰面积呈线性关系,方法的测定下限(10S/N)在0.03～21.2 μg·kg-1之间。在20,100,200 μg·kg-1等3个浓度水平进行加标回收试验,回收率在63.8%~110%之间,测定值的相对标准偏差(n=6)在1.9%~13%之间。
加速溶剂萃取
农药
党参
GC-MS/MS
Accelerated solvent extraction
Pesticide
Radix codonopsis
Abstract
GC-MS/MS was applied to the determination of residual amounts of 69 pesticides in radix codonopsis combined with accelerate solvent extraction. The sample was extracted with acetonitrile as solvent by accelerated solvent extraction. The extract was then purified using Carb/NH2 solid-phase extraction column. The VF-5MS column was used for the GC separation and the multiple reaction-monitoring mode was adopted in MS determination. Linear relationships between peak area and mass concentration of the 69 pesticides were in definite ranges, with lower limits of determination (10S/N) in the range of 0.03-21.2 μg·kg-1. Recovery measured by standard addition method at concentration of 20,100,200 μg·kg-1 and RSD′s (n=6) were in the ranges of 63.8%-110% and 1.9%-13%, respectively.
中图分类号 O657.63
所属栏目 工作简报
基金项目 贵州省科学技术基金(黔科合J字LKG［2013］15号)
收稿日期 2014/4/2
修改稿日期
网络出版日期
作者单位点击查看
联系人作者余磊(824953453@qq.com)
备注余磊(1977-),男,江苏徐州人,高级实验师,硕士,主要研究方向为农药残留分析。
引用该论文: YU Lei,WANG Xing-ning. GC-MS/MS Determination of Residual Amounts of 69 Pesticides in Radix Codonopsis with Accelerate Solvent Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(10): 1232～1238
余磊,王兴宁. 加速溶剂萃取-气相色谱-串联质谱法测定党参中69种农药残留量[J]. 理化检验－化学分册, 2014, 50(10): 1232～1238
共有人对该论文发表了看法，其中：
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】中华人民共和国药典委员会.中华人民共和国药典2010版(一部)［M］.北京: 中国医药科技出版社, 2010: 233-233.
【2】赵春杰,郝桂明,李欢欣.毛细管气相色谱法测定党参中有机氯类农药残留量［J］.中国药学杂志, 2002,37(7): 527-529.
【3】张潇潇,陈晓辉,董婷霞,等.固相萃取-毛细管气相色谱法测定党参、龙胆中15种有机氯农药的残留量［J］.沈阳药科大学学报, 2006,23(12): 776-778.
【4】徐晓琴,李庆玲,黎先春,等.加速溶剂萃取-气相色谱质谱法测定太子参中酰胺类除草剂的含量［J］.分析化学, 2007,35(2): 206-210.
【5】KILJANEK T, NIEWIADOWSKA A, SEMENIUK S. Determination of organophosphorus pesticide residues in the liver by gas chromatography with flame photometric detection［J］. Bull Vet Inst Pulawy, 2011,55: 731-736.
【6】TAN Jun, LIU Xiao-ye, ZHAO Liu-man, et al. Simultaneous and double-quick analysis of organophosphorus pesticide residues in giseng by matrix solid-phase dispersion and high pressure liquid chromatography［J］. Acta Chimica Sinica, 2009,67(20): 2695-2699.
【7】吴胜芳,王利平,刘杨岷,等.加速溶剂萃取-气相色谱串联质谱测定菊花中的3种菊酯类农药残留量［J］.分析试验室, 2008,27(11): 65-67.
【8】苗水,郏征伟,毛秀红,等.气相色谱串联质谱法同时测定黄芪中269种农药残留［J］.中国药学杂志, 2012,47(4): 303-310.
【9】王海涛,张睿,姚燕林,等.高效液相色谱-串联质谱法检测中药材中有机磷农药残留量［J］.分析试验室, 2011,30(1): 72-75.
【10】朱恩圆,贺庆,王峥涛,等.党参化学成分研究［J］.中国药科大学学报, 2011,32(2): 94-95.
【11】胡贝贞,宋伟华,谢丽萍,等.加速溶剂萃取/凝胶渗透色谱-固相萃取净化/气相色谱-质谱法测定茶叶中残留的33种农药［J］.色谱, 2008,26(1): 22-28.
【2】赵春杰,郝桂明,李欢欣.毛细管气相色谱法测定党参中有机氯类农药残留量［J］.中国药学杂志, 2002,37(7): 527-529.
【3】张潇潇,陈晓辉,董婷霞,等.固相萃取-毛细管气相色谱法测定党参、龙胆中15种有机氯农药的残留量［J］.沈阳药科大学学报, 2006,23(12): 776-778.
【4】徐晓琴,李庆玲,黎先春,等.加速溶剂萃取-气相色谱质谱法测定太子参中酰胺类除草剂的含量［J］.分析化学, 2007,35(2): 206-210.
【5】KILJANEK T, NIEWIADOWSKA A, SEMENIUK S. Determination of organophosphorus pesticide residues in the liver by gas chromatography with flame photometric detection［J］. Bull Vet Inst Pulawy, 2011,55: 731-736.
【6】TAN Jun, LIU Xiao-ye, ZHAO Liu-man, et al. Simultaneous and double-quick analysis of organophosphorus pesticide residues in giseng by matrix solid-phase dispersion and high pressure liquid chromatography［J］. Acta Chimica Sinica, 2009,67(20): 2695-2699.
【7】吴胜芳,王利平,刘杨岷,等.加速溶剂萃取-气相色谱串联质谱测定菊花中的3种菊酯类农药残留量［J］.分析试验室, 2008,27(11): 65-67.
【8】苗水,郏征伟,毛秀红,等.气相色谱串联质谱法同时测定黄芪中269种农药残留［J］.中国药学杂志, 2012,47(4): 303-310.
【9】王海涛,张睿,姚燕林,等.高效液相色谱-串联质谱法检测中药材中有机磷农药残留量［J］.分析试验室, 2011,30(1): 72-75.
【10】朱恩圆,贺庆,王峥涛,等.党参化学成分研究［J］.中国药科大学学报, 2011,32(2): 94-95.
【11】胡贝贞,宋伟华,谢丽萍,等.加速溶剂萃取/凝胶渗透色谱-固相萃取净化/气相色谱-质谱法测定茶叶中残留的33种农药［J］.色谱, 2008,26(1): 22-28.
相关信息
