Determination of 31 pesticide residues in Chinese wolfcherry by high performance liquid chromatography-tandem mass spectrometry
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摘要: 建立了高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定枸杞中31种农药残留的方法。枸杞经乙腈提取,Cleant TPH固相萃取柱净化,以C18色谱柱分离待测物,在电喷雾正离子化模式下,采用多反应监测(MRM)检测。结果表明,31种农药在1200μg/L的范围内线性关系良好,相关系数均大于0.995,方法检出限为0.657.1μg/kg,样品添加回收实验的平均回收率为69.7%112.1%,相对标准偏差为5.67%14.27%(n=6)。该方法简单准确,适用于枸杞中31种农药残留的同时检测。
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关键词:
- 高效液相色谱-串联质谱法 /
- 枸杞 /
- 农药残留
Abstract: A method for the simultaneous determination of 31 pesticide residues in Chinese wolfcherry by high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS) was developed. The samples were extracted with acetonitrile, cleaned up by Cleant TPH solid phase extraction column. The resulting samples were separated on a C18 column, and detected by multiple reactions monitoring ( MRM) under the condition of positive mode. The results showed that the linear calibration curves were obtained in the entire range ( 1200 μg/L) for all the above pesticides, with the correlation coefficients higher than 0.995, the detection limit was 0.65 ~ 7.1 μg/kg. For all the samples, the average spiked recoveries ranged 69.7%from 112.1%, and the relative standard deviations ( n = 6) were in the range of 5.67% ~ 14.27%.The method was easy and accurate, and can meet the requirement for the determination of the 31 pesticide residues in Chinese wolfcherry. -
[1] 徐常青, 刘赛, 徐荣, 等.我国枸杞主产区生产现状调研及建议[J].中国中药杂志, 2014, 39 (11) :1979-1984. [2] 陈京闽, 索芳, 王生英.枸杞中对硫磷残留量痕量测定的溶剂微萃取方法的研究[J].中国卫生检验杂志, 2014, 24 (13) :1874-1878. [3] 罗娟, 谢云.高效液相色谱法检测枸杞子中吡虫啉残留量[J].湖北中医药大学学报, 2011, 13 (1) :34-36. [4] 林祥群, 卢春霞, 罗小玲, 等.气相色谱-质谱法测定枸杞中28种农药残留[J].江苏农科科学, 2016, 44 (1) :285-289. [5] 张艳, 王晓菁.液相色谱-串联质谱法测定枸杞中氨基甲酸酯类农药残留量[J].河南农业科学, 2011, 40 (2) :107-110. [6] 陈丽娜, 宋凤瑞, 刘志强.液相色谱-质谱联用技术在中药农药残留分析中的应用进展[J].质谱学报, 2010, 31 (6) :342-353. [7] 梁月香, 王晓菁, 姜瑞, 等.固相萃取-液相色谱串联质谱测定枸杞中有机磷农药残留[J].山东林业科技, 2011 (6) :1-4. [8] 黄何何, 张缙, 徐敦明, 等.Qu ECh ERS-高效液相色谱-串联质谱法同时测定水果中21种植物生长调节剂的残留量[J].色谱, 2014, 32 (7) :707-716. [9] 黄嵩.气质联用和液质联用在农残检测中的应用[J].轻工科技, 2012 (9) :120-121. [10] 林童, 魏玉海, 凤晓博, 等.超高效液相色谱-串联质谱法测定枸杞中常见的5种农药残留[J].现代农药, 2015, 14 (2) :37-39.
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