摘要
目的建立固相萃取柱净化联合气相色谱-串联质谱法(Carb/NH2-solid phase extraction-gas chromatography-tandem mass spectrometric, Carb/NH2-SPE-GC-MS/MS)快速检测79批市售酸枣仁中13种有机氯农药残留,并结合实际污染水平评估有机氯农药的暴露风险。方法样品经乙腈提取,Carb/NH2SPE柱净化后,采用多离子反应监测模式(MRM)对13种农药残留定量监测。结果13种有机氯农药在5~400μg/kg浓度范围内与对应的峰面积呈现良好的线性关系良好(r2>0.996),检出限均低于3μg/kg。本方法应用于79批酸枣仁样品中13种农药的检测,仅1批检出七氯和反式氯丹残留,检出浓度均为0.0025 mg/kg,低于限量规定(0.05mg/kg),慢性暴露风险%ADI为3.95E-03、1.96E-02,表明其无明显健康风险。结论本法操作简单、快速、灵敏度高,可准确监控酸枣仁中有机氯类农药残留。
Objective To establish a method for rapid determination of 13 kinds of organochlorine pesticide residues in 79 batches of commercial Ziziphi Spinosae Semen based on Carb/NH2-solid phase extraction purification and gas chromatography tandem mass spectrometry (GC-MS/MS), and evaluate the exposure risk of organochlorine pesticides according to the actual pollution level. Methods Ziziphi Spinosae Semen samples were extracted with acetonitrile and purified by Carb/NH2 SPE column. The multiple reactions monitoring (MRM) mode was used to detect 13 organochlorine residues. Results The 13 kinds of organochlorine pesticides and their peak area had good linear relationships in the range of 5-400 g/kg (r 2 >1.996), and the limits of detection were all below 3 μg/kg. The method was applied for determination of 13 kinds of pesticides in 79 batches of Ziziphi Spinosae Semens. Among the samples, one batch was found contamination with heptachlor and trans-chlordane, and the detected concentrations were 0.0025 mg/kg (below the limit standards of 0.05 mg/kg). Chronic exposure risk %ADI were 3.95E-03 and 1.96E-02, indicating no significant health risk. Conclusion The Carb/NH2-SPE-GC-MS/MS method is simple, rapid and sensitive, which can accurately and quantitatively analyze the multi-component pesticide residues in Ziziphi Spinosae Semen.
作者
祁伟
豆小文
付延伟
金美奇
谷善勇
范卓文
杨美华
QI Wei;DOU Xiao-Wen;FU Yan-Wei;JIN Mei-Qi;GU Shan-Yong;FAN Zhuo-Wen;YANG Mei-Hua(Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences, Peking Union Medical College, Beijing 100193, China;College of Pharmacy, Heilongjiang University of Chinese Medicine, Harbin 150040, China)
出处
《食品安全质量检测学报》
CAS
2019年第10期2929-2936,共8页
Journal of Food Safety and Quality
基金
国家自然科学基金项目(81703699,81872999)
中国医学科学院医学与健康科技创新工程项目(2016-I2M-1-012,2017-12M-1-013)
科技部重大新药创制科技重大专项(2018ZX09721004-010)~~
关键词
有机氯农药
固相萃取
气相色谱-串联质谱法
多离子反应监测
酸枣仁
organochlorine pesticide
solid phase extraction
gas chromatography-tandem mass spectrometry
multiple reactions monitoring
Ziziphi Spinosae Semen
