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《化学分析计量》 2022年第03期
DOI:10.3969/j.issn.1008-6145.2022.03.013
气相色谱-串联质谱法测定中药材中35种农药残留的样品处理方法
王红梅,石青,王晨,郭贝,郑莉
湖北省普林标准技术服务有限公司,武汉 430050 
The sample treatment method for determination of 35 pesticide residues in Chinese herbal medicine by gas chromatography-tandem mass spectrometry
王红梅,石青,王晨,郭贝,郑莉
Hubei Pulin Standards TechnicaL Services Co., Ltd., Wuhan 430050, China 
摘要:分析对比气相色谱-串联质谱(GC-MS/MS)法测定中药材中35种农药残留的3种样品处理方法,为中药材中农药残留检测提供参考。以乙腈为提取溶剂,样品经高速匀浆提取后,取提取液进行净化处理。比较了基于QuEChERS原则的处理方法、石墨化碳黑-氨基复合固相萃取(GCB-NH2)法和亲水亲油平衡材料固相萃取(HLB)法3种净化方式对中药材中35种农药残留检测的基质效应、色谱峰干扰、回收率等方面的影响。基于QuEChERS原则的处理方法回收率最好,除杀虫脒外其它34种农药回收率均为72.9%~110.9%,但净化效果最差;亲水亲油平衡材料固相萃(HLB)法除油脂和挥发油效果最好,有31种农药回收率均在67.4%~112.5%范围内;石墨化碳黑-氨基复合固相萃取(GCB-NH2)法除色素效果最好,除两种内吸磷外其它33种农药回收率均在68.4%~101.8%范围内。建立了200种中药材样品处理方法数据库,在检测中药材时,可根据不同中药材基质选择相应的样品处理方法。 
Abstract:Three sample treatment methods for the determination of 35 pesticide residues in Chinese herbal medicine by gas chromatography-tandem mass spectrometry(GC-MS/MS) were analyzed and compared, so as to provide reference for the detection of pesticide residues in Chinese herbal medicine. The samples were extracted by acetonitrile in high-speed homogenization. The extraction solution was purified by three methods: treatment method based on QuEChERS principle, graphitized carbon black amino composite solid phase extraction (GCB-NH2) method and hydrophilic lipophilic equilibrium material solid phase extraction (HLB) method. Comparison of three treatment methods was investigated on performances including matrix effect, co-extracted matrix, peak interference and recovery. The recovery rate of the treatment method based on QuEChERS principle was the best, except Chlordimeform, the recovery rates of other 34 pesticides were 72.9%-110.9%, but the purification effect was the worst. HLB had the best effect in removing oil and volatile oil, and the recoveries of 31 pesticides were in the range of 67.4%-112.5%. GCB-NH2 had the best effect in removing pigment, and the recoveries of other 33 pesticides were in the range of 68.4%-101.8% except two kinds of internal phosphorus absorption. The database of sample processing methods of 200 kinds of traditional Chinese herbal medicine was established. When detecting traditional Chinese herbal medicine, the corresponding sample processing methods can be selected according to different matrix of traditional Chinese herbal medicine. 
关键词:气相色谱-串联质谱法;中药材;农药残留;亲水亲油平衡材料固相萃取法;石墨化碳黑氨基复合固相萃取法;QuEChERS原则 
Keywords:gas chromatography-tandem mass spectrometric; Chinese herbal medicine; pesticides residue; HLB; 
本文引用格式:
王红梅,石青,王晨,等.气相色谱-串联质谱法测定中药材中35种农药残留的样品处理方法[J].化学分析计量,2022,31(3):58.
WANG Hongmei,SHI Qing,WANG Chen,et al. The sample treatment method for determination of 35 pesticide residues in Chinese herbal medicine by gas chromatography-tandem mass spectrometry[J]. Chemical Analysis and Meterage,2022,31(3):58. 

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