| 超高效液相色谱-串联质谱法测定粮食中克螨特残留量 |
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| 引用本文： | 张禧庆,李立,娄喜山,付建.超高效液相色谱-串联质谱法测定粮食中克螨特残留量[J].江苏农业学报,2012,28(3):662-666. |
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| 作者姓名： | 张禧庆 李立 娄喜山 付建 |
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| 作者单位： | 1. 烟台杰科检测服务有限公司,山东烟台,265231
2. 中国检验检疫科学研究院,北京,100123 |
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| 摘 要： | 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0.001～0.020 mg/L时,检测方法线性良好,相关系数为0.999 8,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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| 关 键 词： | 超高效液相色谱-串联质谱法 固相萃取 克螨特 粮食 |
Determination of propargite residues in grains by ultra performance liquid chromatography-tandem mass spectrometry |
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| ZHANG Xi-qing
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LI Li
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LOU Xi-shan
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FU Jian.Determination of propargite residues in grains by ultra performance liquid chromatography-tandem mass spectrometry[J].Jiangsu Journal of Agricultural Sciences,2012,28(3):662-666. |
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| Authors: | ZHANG Xi-qing LI Li LOU Xi-shan FU Jian |
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| Institution: | 1(1.Yantai Jieke Inspection Service Co.Ltd.,Yantai 265231,China;2.Chinese Academy of Inspection and Quarantine,Beijing 100123,China) |
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| Abstract: | 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(LOD) was 0.2 μg/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 corn),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. |
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| Keywords: | high performance liquid chromatography-tandem mass spectrometry(UPLC-MS) solid-phase extraction(SPE) propargite grain |
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