高效液相色谱串联质谱法测定人参和金银花中103种农药残留

目的: 应用高效液相色谱串联质谱建立中药材中103种农药的多残留测定法。 方法: 样品用乙腈提取,经凝胶渗透色谱仪和固相萃取柱净化后,以三重四极杆串联质谱在正离子多反应监测(MRM)模式检测,内标法定量。 结果: 各农药在5~250 ng·mL^-1范围内线性良好(r>0.99),三水平回收率在67.0%~102.3%之间,RSD范围0.3%~17.0%,方法检出限在0.19~23.64 μg·kg^-1。 结论: 该法简便、灵敏、准确,适用于中药材中103种农药的多残留测定。

Objective: To establish a method for simultaneous determination of 103 kinds of pesticide residues in Chinese material medica using high-performance liquid chromatography coupled with tandem mass spectrometry. Methods: The samples were extracted with acetonitrile,purified by gel permeation chromatography(GPC)and solid phase extraction(SPE),and then analyzed using LC-MS/MS in multiple reaction monitoring(MRM)mode via positive electrospray ionization using internal standard method. Results: The linearity of the calibration were good in the range of 5250 ng·mL^-1(r>0.99).The recoveries were between 67.0% and 102.3% at three concentration levels,with the relative standard deviations of 0.3%-17.0%.The limits of detection were 0.19-23.64 μg·kg^-1. Conclusion: The method is simple,sensitive and accurate,which can be used for determination of pesticide residues in Chinese material medica.

1 GB 2763-2005.Maximum residue limits for pesticides in food(食品中农药最大残留限量)
2 ChP(中国药典).2010.VolⅠ(一部):Appendix(附录)ⅨQ
3 XUE Jian(薛健),HAO Li-li(郝丽丽),TIAN Jin-gai(田金改),et al.Multiresidue analysis of 29 organochlorine pesticides in Radix Codonopsis(党参中29种有机氯农药的多残留分析).Chin J Pharm Anal(药物分析杂志),2008,28(11):1861
4 ZHI Jian-liang(支建梁),MOU Ren-xiang(牟仁祥),CHEN Ming-xue(陈铭学),et al.Multi-residue determination of 15 phenylurea herbicides in vegetables using solid phase extraction and online post-column ultraviolet decomposition-fluorescent derivatization-high performance liquid chromatography(柱后紫外光解荧光衍生液相色谱法测定蔬菜中残留的15种苯脲除草剂).Chin J Chromatogr(色谱),2008,26(1):93
5 SUN Lei(孙磊),JIN Hong-yu(金红宇),TIAN Jin-gai(田金改),et al.HPLC multi-residue analysis of 13 N-methylcarbamates in traditional Chinese medicines with gel permeation chromatography and postcolumn derivatization(凝胶渗透色谱-柱后衍生高效液相色谱法测定中药材中13种N-甲基氨基甲酸酯农药残留).Chin J Pharm Anal(药物分析杂志),2010,30(4):668
6 SU Jian-feng(苏建峰),LIN Li-feng(林立峰),ZHONG Mao-sheng(钟茂生),et al.Rapid determination of residual amounts of 146 pesticides in yam by gas chromatography-mass spectrometry(山药中146种农药残留的气相色谱-质谱分析方法快速研究).Chin J Pharm Anal(药物分析杂志),2010,30(2):339
7 WANG Ying(王莹),JIN Hong-yu(金红宇),SUN Lei(孙磊),et al.Research of pretreatment platform for simultaneous determination of 198 pesticides in traditional Chinese medicine(中药材中198种农药残留测定样品前处理平台的建立).Chin J Pharm Anal(药物分析杂志),2011,31(12):2199
8 Wang Y,Jin HY,Ma SC,et al.Determination of 195 pesticide residues in Chinese herbs by gas chromatography-mass spectrometry using analyte protectants.J Chromatogr A,2011,1218(2):334
9 LI Yan(李岩),ZHENG Feng(郑锋),WANG Ming-lin(王明林),et al.Rapid screening and confirmation of 156 pesticide residues in concentrated fruit and vegetable juices using liquid chromatography-tandem mass spectrometry(液相色谱-串联质谱法快速筛查测定浓缩果蔬汁中的156种农药残留).Chin J Chromatogr(色谱),2009,27(2):127
10 CAO Jing(曹静),PANG Guo-fang(庞国芳),WANG Ming-lin(王明林),et al.Determination of 215 pesticide residues in ginger using liquid chromatography coupled with electrospray ionization tandem mass spectrometry(液相色谱-电喷雾串联质谱法测定生姜中的215种农药残留).Chin J Chromatogr(色谱),2010,28(6):579
11 Ferrer I,Thurman EM,Zweigenbaum JA.Screening and confirmation of 100 pesticides in food samples by liquid chromatography/tandem mass spectrometry.Rapid Commun Mass Spectrom,2007,21(23):3869
12 Zhang K,Wong JW,Yang P,et al.Multiresidue pesticide analysis of agricultural commodities using acetonitrile salt-out extraction,dispersive solid-phase sample clean-up,and high-performance liquid chromatography-tandem mass spectrometry.J Agric Food Chem,2011,59(14):7636