固相萃取-高效液相色谱-串联质谱法同时测定鸡蛋中42种农药残留

Simultaneous determination of 42 pesticide residues in eggs by solid phase extraction method combined with high performance liquid chromatography-tandem mass spectrometry

中文关键词:  鸡蛋  农药残留  固相萃取  高效液相色谱-串联质谱法

英文关键词:eggs  pesticide residues  solid phase extraction  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立固相萃取-高效液相色谱-串联质谱法同时测定鸡蛋中42种农药残留的检测方法。方法 样品加水分散后, 用乙腈提取, PRiME HLB固相萃取柱进行净化处理, 采用Shim-pack XR-ODSⅡ色谱柱(75 mm× 2.0 mm, 2.2 μm)分离, 5 mmol/L乙酸铵水溶液(A)-甲醇溶液(B)为流动相, 进行梯度洗脱; 质谱法选择电喷雾离子源ESI, 正负离子分段扫描, 多反应监测(multiple reaction monitoring, MRM)模式检测, 基质匹配标准溶液外标法定量。结果 42种农药的峰面积与质量浓度在0.1~2.0 ng/mL范围内呈现良好的线性关系, 相关系数r均大于0.994; 方法检出限为0.04~0.4 μg/kg, 定量限为0.1~1.0 μg/kg。在1.0、2.0、5.0、10 μg/kg 4个添加水平下, 42种农药平均加标回收率为61.0%~118.5%, 相对标准偏差为0.8%~9.9%。结论 该方法具有操作简单、分析时间短、试剂用量少、灵敏度高且重复性好等特点, 适用于鸡蛋中农药残留的高通量快速检测分析。

英文摘要:

      Objective To establish a method for simultaneous determination of 42 pesticide residues in eggs by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were dispersed in water and extracted with acetonitrile, and purified by PRiME HLB. The analytes were separated on a Shim-pack XR-ODSⅡ column (75 mm×2.0 mm, 2.2 μm) with 5 mmol/L ammonium acetate aqueous solution (A)-methanol solution (B) as the mobile phase using gradient elution. The identifications were achieved by mass spectrometry using electrospray ionization with positive and negative ions piecewise scanning mode in the multiple reaction monitoring (MRM). The quantifications were performed by matrix-matched extremely standard method. Results There was a good linear relationship between peak area and mass concentration of 42 pesticides in the range of 0.1?2.0 ng/mL, and correlation coefficients were all greater than 0.994. Limits of detection for pesticide residues was 0.04?0.4 μg/kg, and limits of quantitation was 0.1?1.0 μg/kg. The average standard recoveries of 42 pesticides were 61.0%?118.5%, and the relative standard deviations were 0.8%?9.9% at the 4 additive levels of 1.0, 2.0, 5.0, 10 μg/kg. Conclusion This method is simple, fast, sensitive, accurate and reproducible, which is suitable for rapid high-throughput detection of pesticide residues in eggs.