中国药品标准2024,Vol.25Issue(3) :251-256.DOI:10.19778/j.chp.2024.03.006

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

张万青 刘芫汐 陈高翩 朱慧茹 朱玉芳 刘潇潇
中国药品标准2024,Vol.25Issue(3) :251-256.DOI:10.19778/j.chp.2024.03.006

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

张万青 1刘芫汐 2陈高翩 1朱慧茹 1朱玉芳 1刘潇潇1
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作者信息

  • 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
  • 折叠

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-C18(2.1 mm × 100 mm,2.7 μm);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.

Abstract

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 hydro-phile-lipophile balance(HLB)solid-phase extraction method,and the residual amounts of carbofuran,3-carboxyl-carbofuran,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-C18(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 QuECh-ERS 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 recommen-ded 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

Key words

pesticide residues/QuEChERS/HLB material/Angelicae Sinensis Radix/ChrysanthemI Flos/Lych Fructus/Astragali Radix/Lonicerae Japonicae Flos

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出版年

2024
中国药品标准
国家药典委员会

中国药品标准

影响因子:0.372
ISSN:1009-3656
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