色谱

色谱 ›› 2016, Vol. 34 ›› Issue (6): 577-582.DOI: 10.3724/SP.J.1123.2016.01034

• 研究论文 • 上一篇    下一篇

QuEChERS-高效液相色谱-串联质谱法测定植物源食品中氯啶菌酯和丙炔恶草酮残留

粟有志, 李芳, 于晶晶, 李艳美, 雷红琴, 罗琼   

  1. 伊犁出入境检验检疫局综合技术服务中心, 新疆 伊宁 835000
  • 收稿日期:2016-01-28 出版日期:2016-06-08 发布日期:2013-01-23
  • 通讯作者: 粟有志
  • 基金资助:

    新疆维吾尔自治区自然科学基金项目(201442137-23)

Determination of triclopyricarb and oxadiargyl residues in vegetative foods by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

SU Youzhi, LI Fang, YU Jingjing, LI Yanmei, LEI Hongqin, LUO Qiong   

  1. Comprehensive Technical Service Centre of Yili Entry-Exit Inspection and Quarantine Bureau, Yining 835000, China
  • Received:2016-01-28 Online:2016-06-08 Published:2013-01-23
  • Supported by:

    Natural Science Foundation of the Xinjiang Uygur Autonomous Region (No. 201442137-23).

PDF

128

被引次数

7

摘要：

建立了QuEChERS前处理-高效液相色谱-串联质谱(HPLC-MS/MS)同时检测植物源食品中氯啶菌酯和丙炔恶草酮残留量的分析方法。样品经酸化乙腈提取,采用乙二胺-N-丙基硅烷(PSA)和氨基(NH2)吸附剂净化。以0.1%(v/v)甲酸水(含2 mmol/L乙酸铵)-甲醇(2:8, v/v)为流动相,在0.25 mL/min流速下等度洗脱,采用C18色谱柱分离,电喷雾正离子电离(ESI+)、多重反应监测(MRM)模式质谱检测。以保留时间和特征离子对(母离子和两个碎片离子)信息比较进行定性,基质匹配外标法定量。结果表明:在葡萄、葡萄干、马铃薯、大米、番茄、油菜籽6种基质中,氯啶菌酯和丙炔恶草酮在各自线性范围内线性关系良好(相关系数r2均大于0.996)。氯啶菌酯的定量限(LOQ)(以S/N≥10计)为0.5 μg/kg,丙炔恶草酮的定量限为1.0 μg/kg。在1、2、10倍LOQ 3个添加水平下,氯啶菌酯的平均回收率为71.6%~112.1%,相对标准偏差为2.6%~12.1%;丙炔恶草酮的平均回收率为77.6%~118.8%,相对标准偏差(RSD)为3.6%~14.3%。该方法高效快捷、灵敏、准确,适用于植物源性食品中氯啶菌酯和丙炔恶草酮的快速检测。

关键词: QuEChERS, 丙炔恶草酮, 高效液相色谱-串联质谱, 氯啶菌酯, 植物源食品

Abstract:

A method for the simultaneous determination of triclopyricarb and oxadiargyl residues in vegetative foods was developed using QuEChERS-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was extracted with acidic acetonitrile, and then cleaned up by primary secondary amine (PSA) and NH2 adsorbents. The analytes were separated on a C18 column with isocratic gradient elution of 0.1%(v/v) formic acid in water (containing 2 mmol/L ammonium acetate)-methanol (2:8, v/v) at a flow rate of 0.25 mL/min. The mass spectrometry was carried out with electrospray positive ion source (ESI+) in multiple reaction monitoring (MRM) mode. The qualitative analysis was based on the retention times and characteristic ion pairs consisting of one parent ion and two fragment ions, and the quantitative analysis was carried out by matrix-matched external standard method. The results showed that calibration curves had good linearities for triclopyricarb and oxadiargyl, and the correlation coefficients (r2) were larger than 0.996; the limits of quantification (LOQs, S/N≥10) of triclopyricarb in the six matrices (grape, raisin, potato, rice, tomato, rapeseed) were 0.5 μg/kg, and the LOQs of oxadiargyl in the six different matrices were 1.0 μg/kg. When the articles were spiked with three levels of analytes (1×LOQ, 2×LOQ and 10×LOQ), the recoveries of triclopyricarb were from 71.6% to 112.1% with the RSDs from 2.6% to 12.1%; and the recoveries of oxadiargyl were from 77.6% to 118.8% with the RSDs from 3.6% to 14.3%. The method is highly effective, sensitive, accurate, and is suitable for the monitoring of triclopyricarb and oxadiargyl in vegetative foods.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), oxadiargyl, QuEChERS, triclopyricarb, vegetative foods

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