超高效液相色谱-串联质谱法测定中草药中氨基甲酸酯类农药残留量

目的: 结合固相萃取技术,克服了中草药样品中复杂的基质干扰问题,建立超高效液相色谱-串联质谱(UPLC-MS/MS)法检测中药材中15种氨基甲酸酯类杀虫剂的残留量。 方法: 样品中残留的农药经乙腈提取,PSA固相萃取柱净化后,采用UPLC-MS/MS法进行测定。 结果: 15种农药在其各自的浓度范围内,线性关系良好,相关系数在0.995～0.999之间。在定量限(LOQ)、5倍定量限和10倍定量限3个添加浓度水平,平均加标回收率在61.8%～98.1%之间;RSD在1.8%～14.8%之间。 结论: 该方法操作简便,净化效果好,灵敏度高,可为中药材中氨基甲酸酯类杀虫剂污染状况调查提供检测方法支持。

Objective: An ultra performance liquid chromatography-tandem mass spectrometric method was developed for the determination of 15 carbamate pesticides in traditional Chinese medicine. Method: Pesticides were extracted with acetonitrile,cleaned up by PSA solid phase extraction column,and then analyzed by UPLC-MS/MS. Result: The standard calibration curves for 15 carbamate pesticides showed high correlation coefficient (0.995-0.999) over their respective concentration range.The average recovery of 15 carbamate pesticides at the three fortification levels (LOQ,5 LOQ and 10 LOQ) was between 61.8% and 98.1% with the relative standard deviation between 1.8% and 14.8%. Conclusion: It was indicated that the method developed in this study is easier,more sensitive and has a better purification effect.So,this method can be further applied to investigate the contamination status of traditional Chinese medicine by the carbamate pesticides.

[1] WAN Yi-qun (万益群),LI Shen-jie (李申杰),FU Gui-qin (付贵琴).Determination of organophosphorous and carbamates pesticides residues in Chinese herbal medicine (中草药中有机磷及氨基甲酸酯类农药残留量的GC-MS测定). Chin J Anal Lab (分析实验室),2007,26 (6):81
[2] LIU Li-ping(刘丽萍).Determination of carbamates pesticides residues in vegetables by HPLC with postcolumn derivatization (高效液相色谱柱后衍生法测定蔬菜中氨基杀虫剂农药残留).China Pract Med (中国实用医药),2008,3(8):116
[3] GAN Feng-juan (甘凤娟),CHEN Yan-meng (陈砚朦),LI Yue-huan (李月欢),et al.Determination of residual carbamates pesticides by HPLC with postcolumn fluorescent derivatization(高效液相色谱-柱后衍生荧光法检测氨基甲酸酯类农药残留量).Chin J Health Lab Technol (中国卫生检验杂志),2005,15(12):1460
[4] NY/T 761.3-2004
[5] LIANG Qi (梁祈),WEI Xue-fang(魏雪芳).Determination of organonitrogen pesticides residues in Chinese medicine crop Radix Astragali by high performance liquid chromatography (中药材黄芪中有机氮农药残留量的液相色谱检测方法). J Instrum Anal (分析测试学报),2000,19(2):45
[6] DONG Shun-ling (董顺玲),HU Jia-zhi (胡家炽),HE Zhi-qiang (何志强),et al.RP-HPLC determination of residual of aldicarb,carbofuran and carbaryl in Chinese crude drugs (中药材中氨基甲酸酯类农药残留量的反相高效液相色谱法).Chin J Pharm Anal (药物分析杂志),2002,22 (3):178
[7] 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
[8] CHEN Xiao-hong (陈晓红),LI Xiao-ping (李小平),JIN Mi-cong (金米聪).Determination of the residues of carbamate pesticides in vegetables by liquid chromatography mass spectrometry (蔬菜中氨基甲酸酯类农药残留的HPLC/MS 测定研究).Chin J Health Lab Technol (中国卫生检验杂志),2006,16(9):1041
[9] Kmellár B,Fodor P,Pareja L,et al.Validation and uncertainty study of a comprehensive list of
[160] pesticide residues in multi-class vegetables by liquid chromatography–tandem mass spectrometry.J Chromatogr A,2008,1215:37
[10] ZHAO Ying (赵颖),PAN Wei (潘伟),JIN Yan (金雁),et al.Determination of
[19] carbamate pesticides residues in fish vegetables by UPLC-MS/MS (UPLC-MS/MS 同时测定蔬菜中19 种氨基甲酸酯类药物残留). Fujian Anal Test (福建分析测试),2009,4:57
[11] MAO Jiang-sheng (毛江胜),MENG Jing-jing (孟静静),ZHAO Shan-cang (赵善仓),et al.Determination of carbofuran,aldicarb and its metabolite residues in grains by UPLC-MS/MS (超高效液相色谱串联质谱法测定粮谷中克百威、涕灭威及其代谢物的残留量).Chin J Anal Chem (分析化学),2009,37(12):1857
[12] XU Yuan-jin (徐远金),LI Yong-ku (李永库).HPLC-MS analysis for contents of residual carbamate pesticides in a variety of Chinese herbal medicines (中药材中氨基甲酸酯类农药的高效液相色谱-质谱分析).Phys Test Chem Anal Part B (Chem Anal) (理化检验-化学分册),2006,42 (11):877