| 高效液相色谱串联质谱测定武夷岩茶中草甘膦残留量的方法探讨 |
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| 引用本文： | 衷兴旺.高效液相色谱串联质谱测定武夷岩茶中草甘膦残留量的方法探讨[J].山东化工,2014(7):70-72. |
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| 作者姓名： | 衷兴旺 |
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| 作者单位： | [1]武夷山市质量计量检测所,福建武夷山354300; [2]武夷山市茶叶产品质量检验所,福建武夷山354300 |
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| 基金项目： | 国家质检总局科技计划项目（2013QK311） |
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| 摘 要： | 采用高效液相色谱串联质谱建立了武夷岩茶样品中草甘膦的残留量的测定方法。样品经水固相萃取和茶叶专用萃取柱(TPT)净化后,在硼酸盐缓冲液中与9-芴甲基氯甲酸酯(FMOC-Cl)进行衍生化反应,以1%乙酸铵溶液和乙腈为流动相,质谱检测采用电喷雾正离子化模式和多反应监测模式。结果表明,草甘膦在1~10 ng/mL范围内线性良好,线性相关系数r=0.998。通过对空白武夷岩茶样品进行4个加标水平的添加回收实验(n=5),草甘膦的平均回收率和相对标准偏差(RSD)分别为87.3%~98.0%和3.46~5.12。
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| 关 键 词： | 液相色谱-串联质谱 草甘膦 衍生反应 |
Characterize Glyphosate Residues in Wuyi Rock Tea Using HPLC Tandem Mass Spectrometric Method |
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| Zhong Xingwang.Characterize Glyphosate Residues in Wuyi Rock Tea Using HPLC Tandem Mass Spectrometric Method[J].Shandong Chemical Industry,2014(7):70-72. |
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| Authors: | Zhong Xingwang |
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| Affiliation: | Zhong Xingwang ( 1. Quality and Measurement Research Institution of Wuyishan,Wuyishan 354300, China; 2. The Product Quality Inspection Institute of Wuyishan, Wuyishan 354300, China) |
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| Abstract: | A method for determination of glyphosate residues in Wuyi rock tea was developed using high performance liquid chromatography tandem mass spectrometry method. The procedure is as follow, the glyphosate were extracted with water from samples, and purified using TPT. Then derivatization reaction was clone in borate buffer with fluorenylmethylchloroformate （FMOC -C1）. Using 1% solution of ammonium acetate and aeetonitrile as the mobile phase, mass spectrometry using electrospray ionization in positive ionization mode and multiple reaction monitoring mode. The results showed that the linear correlation coefficient r = 0. 998 when glyphosate is betweenlng - 10ng/mL. Wuyi blank samples were used in added recovery experiment at four spiked levels（n =5）, the average recovery of glyphosate were 87. 3% to 98.0%. The relative standard deviation （RSD） were 3.46 to 5.12. |
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| Keywords: | HPLC - tandem mass spectrometry glyphosate derivative reaction |
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