作者：周冰¹, 安国荣¹, 朱琳¹, 阎娥²

作者单位：1. 青海省地质矿产测试应用中心，青海 西宁 810000;
2. 青海师范大学，青海 西宁 810000

关键词：高效液相色谱串联质谱;樱桃;啶菌噁唑;农药残留

摘要：

建立高效液相色谱串联质谱（HPLC-MS/MS）测定樱桃和土壤中啶菌噁唑、乙霉威、噻菌灵、嘧菌酯残留的分析方法。样品以乙腈溶液提取, 经混合盐盐析，离心后膜过滤，以0.2%甲酸溶液和乙腈作为流动相进行梯度洗脱，通过电喷雾离子源正离子检测模式和多重反应监测模式测定，采用外标法定量分析。结果表明4种农药的进样质量浓度在0.0001~0.0100 mg/L范围内，其峰面积与质量浓度呈现良好的线性关系，r²>0.993，且4种农药的检测限均优于7.34×10^–5 mg/kg。分别在0.1，1，10 μg/kg 3个浓度水平下做加标回收率验证，回收率在82.44%~104.54%之间，相对标准偏差均小于4.92%。该方法简单、快速、准确， 适合用于樱桃和土壤中啶菌噁唑等农药残留的定性和定量检测。

Determination of insecticides against Botrytis cinerea in cherry and soil using LC-MS/MS method
ZHOU Bing¹, AN Guorong¹, ZHU Lin¹, YAN E²
1. Qinghai Province Geology and Mineral Testing and Application Center, Xining 810000, China;
2. Qinghai Normal University, Xining 810000, China
Abstract: To establish a HPLC-MS /MS method for the determination of residues of oxazole, diethofencarb, thiabendazole and azoxystrobin in cherry and soil. The samples were extracted with acetonitrile solution, salted out with mixed salt, filtered by membrane after centrifugation, and gradient elution was performed with 0.2% formic acid solution and acetonitrile as mobile phase. The positive ion detection mode and multiple reaction monitoring mode of electrospray ion source were used for quantitative analysis using external standard method. Within the range of 0.0001 mg/L to 0.0100 mg/L, there was a good linear relationship between the mass concentration of the four pesticides and the corresponding peak area, r²>0.993, and the detection limits were all lower than 7.34×10^–5 mg/kg. The average recoveries at 0.1, 1 and 10 μg/kg levels were 82.44% to104.54%, and all RSD were less than 4.92%. The method is suitable for the qualitative and quantitative detection of pesticide residues such as oxazole in cherry and soil for its simple, rapid and accurate personality.
Keywords: LS-MS/MS;cherry;oxazoles;pesticide residues
2022, 48(2):80-85  收稿日期: 2020-11-27;收到修改稿日期: 2021-01-13
基金项目: 青海省科技成果转化专项（2019-SF-139）
作者简介: 周冰(1981-),女,宁夏银川市人,工程师,研究方向为土壤、水质、生物、固废的无机和有机分析测试等
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