高效液相色谱串联质谱法快速检测淫羊藿药材中47种农药残留  

Rapid Detection of 47 Pesticide Residues in Epimedii Folium by HPLC - MS / MS

作　　者：章会琼 杨琴[1] 蒲雪 刘明容 ZHANG Huiqiong;YANG Qin;PU Xue;LIU Mingrong(The Hospital of Traditional Chinese Medicine of Leshan,Leshan,Sichuan,China 614000)

机构地区：[1]四川省乐山市中医医院,四川乐山614000

出　　处：《中国药业》2023年第22期103-107,共5页China Pharmaceuticals

摘　　要：目的 建立快速检测淫羊藿药材中47种农药残留的高效液相色谱串联质谱(HPLC-MS/MS)法。方法 色谱条件,色谱柱为Kromasil 100-5 C_(18)柱(150 mm×3.9 mm,5μm),流动相为乙腈-0.1%甲酸水溶液(梯度洗脱),流速为0.4 mL/min,柱温为40℃,进样量为10μL;质谱条件,扫描模式为多反应监测(MRM)模式,电喷雾离子源正离子模式(ESI+),雾化气温度为450℃,气帘气压力为30 psi,碰撞气压力为5 psi,离子源电压为4 500 V,辅助气1,2压力均为30 psi。结果 47种农药对照品质量浓度均在2~20 ng/mL范围内与峰面积线性关系良好(r>0.997);检测限为0.04~6.50μg/kg;精密度、稳定性试验结果的RSD均小于4.0%;47种农药的加样回收率分别为72.23%~96.33%,RSD为1.40%~4.90%(n=9);基质效应考察结果表明,40种农药存在负基质效应,且38种农药的基质效应不可忽略。25批药材样品中有10批检出农药(共4种)残留。结论 该方法具有分析速度快、灵敏度高、准确度高、高通量等特点,适用于淫羊藿药材中47种农药残留的快速检测。Objective To establish a high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for the rapid detection of 47 pesticide residues in Epimedii Folium.Methods For chromatographic conditions,the chromatographic column was Kromasil 100-5 C_(18) column(150 mm×3.9 mm,5μm),the mobile phase was acetonitrile-0.1%formic acid aqueous solution(gradient elution),the flow rate was 0.4 mL/min,the column temperature was 40℃,and the injection volume was 10μL.For mass spectrum conditions,the scanning mode was multiple reaction monitoring(MRM)mode,the electro-spray ionization with positive ion(ESI+)was adopted,the atomizing gas temperature was 450℃,the curtain gas pressure was 30 psi,the collision gas pressure was 5 psi,the ion source voltage was 4500 V,and the auxiliary gas 1 and 2 pressures were both 30 psi.Results The linear range of 47 pesticide reference was 2-20 ng/mL(r>0.997).The limit of detection was in the range of 0.04 to 6.50μg/kg.The RSDs of precision and stability tests were both lower than 4.0%.The recovery rates of 47 pesticides were in the range of 72.23%to 96.33%with RSDs of 1.40%to 4.90%(n=6).The investigation of matrix effects showed that 40 pesticides had negative matrix effects,and those of 38 pesticides could not be ignored.Four pesticide residues were detected in 10 out of 25 batches of medicinal samples.Conclusion This method is fast,sensitive,accurate and high-throughput,which is suitable for the rapid detection of 47 pesticide residues in Epimedii Folium.

关 键 词：淫羊藿 农药残留 含量测定 高效液相色谱串联质谱法 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]