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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0.5μg／kg，丙炔恶草酮的定量限为1.0μg／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。

A method for the simultaneous determination of triclopyricarb and oxadiargyl resi-dues in vegetative foods was developed using QuEChERS-high performance liquid chromatogra-phy-tandem mass spectrometry( HPLC-MS/MS). The sample was extracted with acidic acetoni-trile,and then cleaned up by primary secondary amine( PSA)and NH2 adsorbents. The ana-lytes 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 reten-tion 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.