同位素内标-超高效液相色谱-串联质谱法快速测定植物性食品中11种杀菌剂残留量
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(安徽省疾病预防控制中心,安徽 合肥 230601)

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赵紫微 女 主管技师 研究方向为食品安全的理化检验 E-mail:zhaoziwei0603@163.com

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Rapid determination of 11 fungicide residues in plant foods by ultra-high performance liquid chromatography-tandem mass spectrometry with isotope internal standards
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(Anhui Center for Disease Control and Prevention, Anhui Hefei 230601, China)

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    摘要:

    目的 建立快速同时测定植物性食品中11种杀菌剂残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。方法 植物性食品经乙腈提取,经匀浆和高速离心后采用QuEChERS试剂净化,用HSS T3色谱柱(2.1 mm×100 mm,1.7 μm)进行分离,以0.1%甲酸水溶液-乙腈为流动相,电喷雾电离,正离子扫描(ESI+),多反应监测(MRM)模式检测目标物,同位素内标法定量。结果 11种杀菌剂在0.1~50.0 μg/L浓度范围内具有良好的线性,相关系数(r2)均大于0.999 1,检出限为0.2~2.0 μg/kg,平均回收率范围为63.1%~116.3%,相对标准偏差(RSD)均小于12.1%。结论 该方法操作简单快速、灵敏度高、准确性好,适用于对大批量植物性食品中多种杀菌剂的快速测定。

    Abstract:

    Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for rapid and simultaneous determination of 11 fungicide residues in plant foods. Methods The plant foods were extracted by acetonitrile with homogenate and high speed centrifugation and purified by QuEChERS reagent. The 11 fungicides were separated on a HSS T3 column (2.1 mm×100 mm,1.7 μm) with 0.1% formic acid water-acetonitrile as mobile phase. The identifications were performed by electrospray ionization with positive scanning mode(ESI+) under the multiple reaction monitoring (MRM), and the internal standard method was used to quantify the analytes. Results The calibration curves of the 11 kinds of fungicides showed good linearity in the concentration range of 0.1-50.0 μg/L, with the correlation coefficient (r2) above 0.999 1. The detection limit was 0.2-2.0 μg/kg. The average recoveries were between 63.1% and 116.3%, and the relative standard deviations (RSD) were less than 12.1%. Conclusion The method was simple, rapid, sensitive and accurate. It was suitable for rapid determination of various fungicides in a large number of plant foods.

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赵紫微,刘柏林,谢继安,王秀莉,单晓梅.同位素内标-超高效液相色谱-串联质谱法快速测定植物性食品中11种杀菌剂残留量[J].中国食品卫生杂志,2019,31(1):22-28.

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  • 收稿日期:2018-11-19
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  • 在线发布日期: 2019-03-22
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