不同前处理方法对5种中药农药残留量检测的影响  

Effect of different pretreatment methods on the detection of pesticide residues in five traditional Chinese medicines

作　　者：张万青 刘芫汐 陈高翩 朱慧茹 朱玉芳[1] 刘潇潇[1] ZHANG Wanqing;LIU Yuanxi;CHEN Gaopian;ZHU Huiru;ZHU Yufang;LIU Xiaoxiao(Guangdong Institute for Drug Control,Guangzhou 510663,China;National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]广东省药品检验所,广州510663 [2]中国食品药品检定研究院,北京100050

出　　处：《中国药品标准》2024年第3期251-256,共6页Drug Standards of China

基　　金：广东省药品监督管理局科技创新项目(2024ZDZ14)。

摘　　要：目的:研究分析不同前处理方法对当归、菊花、枸杞子、黄芪、金银花中农药残留测定结果的影响。方法:样品分别经QuEChERS法和高速匀浆结合亲水亲油平衡(HLB)材料固相萃取法处理,采用超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定克百威、3-羧基克百威、甲拌磷、甲拌磷砜、甲拌磷亚砜、甲基异柳磷等5种农药残留量。采用超高效液相色谱柱Agilent Poroshell 120 SB-C_(18)(2.1 mm×100 mm,2.7μm);采用梯度洗脱方式,水相为含5 mmol·L^(-1)甲酸铵的0.1%甲酸溶液,有机相为含5 mmol·L^(-1)甲酸铵的0.1%甲酸溶液-乙腈(体积比5∶95);柱温为35℃;质谱分析中以电喷雾离子源正离子模式扫描,多反应监测模式检测。结果:QuEChERS法和HLB固相萃取法测得结果偏差在9.09%~55.56%之间。结论:中药农药残留量检测前处理方法的选定,建议以阳性样本的测定数据为评价指标与依据,选择测定值较高、提取效率高的方法。Objective:To study effects of different pretreatment methods on the detection of pesticide residues in Angelicae Sinensis Radix,ChrysanthemI Flos,Lych Fructus,Astragali Radix and Lonicerae Japonicae Flos.Methods:The samples were treated with QuEChERS method and high-speed homogenization combined with hydrophile-lipophile balance(HLB)solid-phase extraction method,and the residual amounts of carbofuran,3-carboxylcarbofuran,phorate,phorate sulfone,phorate sulfoxide,and methyl isoflurophos were simultaneously determined using UHPLC-MS/MS.With a gradient elutionof 0.1%formic acid solution containing 5 mmol·L^(-1)ammonium formate and t 0.1%formic acid solution containing 5 mmol·L^(-1)ammonium formate-acetonitrile(volume ratio of 5∶95),Ultra-performance liquid chromatography column Agilent Poroshell 120 SB-C_(18)(2.1 mm×100 mm,2.7μm)was used at 35℃and the electrospray ion source was scanned in the positive ion mode and detected in the multiple reaction monitoring mode in mass spectrometry.Results:The deviation of the results measured by QuEChERS method and HLB solid-phase extraction method was between 9.09%-55.56%.Conclusion:In the selection of the pretreatment method for the detection of pesticide residues in traditional Chinese medicine,it is recommended to take the measurement data of positive samples as the evaluation index and basis,and choose the method with higher measurement value and high extraction efficiency.

关 键 词：农药残留 QUECHERS 亲水亲油平衡材料 当归 菊花 枸杞子 黄芪 金银花 

分 类 号：R921.2[医药卫生—药学]