液相色谱-串联质谱法测定水果中6种植物生长调节剂残留量
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(成都市疾病预防控制中心,四川 成都 610041)

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王炼 男 副主任技师 研究方向为有机污染物残留分析E-mail:septwolvesnjwl@163.com

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中国博士后面上项目(2012M521703)


Determination of 6 plant growth regulator residues in fruits by liquid chromatography-tandem mass spectrometry
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(Chengdu Centre for Disease Control and Prevention,Sichuan Chengdu 610041,China)

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    摘要:

    研究同位素内标-液相色谱-串联质谱测定水果中6种植物生长调节剂的方法。方法 样品经含1%乙酸的乙腈提取,采用Welch Xtimate C18色谱柱(2.1 mm×100 mm,3 μm),乙腈-0.01%氨水(含2 mmol/L乙酸铵)为流动相,梯度洗脱,多反应离子监测(MRM)模式,分段ESI+与ESI-扫描方式检测。结果 0.6、10和50 μg/kg三个浓度的样品加标试验,回收率为80.1%~115.0%,相对标准偏差为4.3%~9.9%,定量限和检出限分别在0.2~4.0和0.06~1.5 μg/kg。结论 建立的分析方法简便、准确、灵敏,满足食品中农药最大残留限量要求。

    Abstract:

    To establish a method for determination of 6 plant growth regulator residues in fruits by liquid chromatography-tandem mass spectrometry using the isotope internal standard.Methods The sample was extracted by acetic acid in acetonitrile and homogenized. After dehydration reagent treatment, the sample was centrifugated and cleaned-up by dispersive solid phase extraction tube. The supernatant was detected by vortex mixing and centrifugation. The conditions of elution for mobile phase and analysis for mass spectrometry were optimized. Results The recovery test of the spiked sample was used with 3 concentrations, 0.6,0 and 50 μg/kg. The spiked sample recoveries were at 80.1%-115.0% and the relative standard deviations of detection were at 4.3%-9.9%. The limits of quantification and detection were 0.2-4.0 and 0.06-1.5 μg/kg.Conclusion The method is simple, accurate, sensitive and it can meet the determination requirements of pesticide residues in foods.

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王炼,骆春迎,张礼春,余辉菊.液相色谱-串联质谱法测定水果中6种植物生长调节剂残留量[J].中国食品卫生杂志,2016,28(4):451-456.

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  • 收稿日期:2016-01-07
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  • 在线发布日期: 2016-08-18
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