首页> 中文期刊> 《江苏农业学报》 >超高效液相色谱-串联质谱法测定粮食中克螨特残留量

超高效液相色谱-串联质谱法测定粮食中克螨特残留量

             

摘要

The techniques of solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry were used to develop a method for determination of propargite residues in grains. The samples were dipped into water for 30 min, extracted using acetonitrile by ultrasonic method, and then purified by C18 and NH2 solid-phase extraction column. The target compound was separated on a C18 column with a gradient elution of 0. 1% formic acid aqueous solution (including 5 mmol/L ammonium acetate) and acetonitrile (including 0.1% formic acid) as mobile phase. The identification and quantification were conducted using electrospray ionization in positive ion mode (ESI+) with multiple reactions monitoring ( MRM), and were confirmed by external standard method. The linearity of method was good between 1.0 μg/L and 20.0 μg/L propargite (r2 = 0.999 8). The limit of detection (WD) was 0.2 |xg/kg, and the limit of quantification (LOQ) was 1.0 μg/kg. The recoveries were in the range of 60. 5%-90.2% at three spiked levels (1 μg/kg, 2 μg/kg and 5 μg/kg) in six grains (wheat, barley, oat, rice, black rice and com), and the relative standard deviations (RSD) were in the range of 1.7%-13.7%. The method works well with no interference, and is suitable for the quantitative determination of propargite residues in grains.%为了建立粮谷中克螨特残留量的测定方法,采用了固相萃取-超高效液相色谱-串联质谱法进行检测.样品加入适量水浸润后,乙腈超声提取,液液萃取后,经碳十八和氨基固相萃取柱净化,超高效液相色谱串联质谱多反应监测测定,外标法定量.结果显示,克螨特在0.001~0.020mg/L时,检测方法线性良好,相关系数为0.9998,检测限为0.2μg/kg,定量限为1.0μg/kg.对小麦、大麦、燕麦、大米、黑米、玉米6种粮谷进行3个水平的添加回收试验(1μg/kg、2μg/kg、5μg/kg),结果回收率在60.5%与90.2%之间,相对标准偏差为1.7%~13.7%.运用该方法检测粮谷时基本没有干扰现象,适用于粮谷中克螨特残留的测定.

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