高效液相色谱-串联质谱法检测茶叶中痕量草胺膦、草甘膦及其代谢物氨甲基膦酸残留
赵春华,左于一菲,孙倩
诺安实力可商品检验(青岛)有限公司,山东青岛 266011
Determination of trace glufosinate, glyphosate and its metabolites residue in tea by HPLC-MS/MS
赵春华,左于一菲,孙倩
Sino Silliker Testing Services (Qingdao) Co., Ltd., Qingdao 266011, China
摘要:建立高效液相色谱-串联质谱法测定茶叶中除草剂草胺膦、草甘膦及其代谢物氨甲基膦酸残留的方法。以纯水提取茶叶中的草胺膦、草甘膦、氨甲基膦酸,用二氯甲烷、阴离子交换固相萃取柱净化、富集,以0.25 mol/L碳酸氢钠溶液洗脱,然后直接采用1%芴甲氧羰酰氯进行衍生,衍生时间为5 min,用反相液相色谱柱分离,以电喷雾正离子模式,多反应模式(MRM)检测。草胺膦、草甘膦、氨甲基膦酸的质量浓度在0~20 μg/L范围内均具有良好的线性,线性相关系数大于0.995,方法定量限为0.01 mg/kg。在不同茶叶基质中,0.01,0.025,0.05 mg/kg三水平的平均添加回收率为94.0%~116.0%,测定结果的相对标准偏差为3.5%~7.1%(n=6)。该方法操作简便,灵敏度与准确度高,满足茶叶样品中草胺膦、草甘膦及其代谢物氨甲基膦酸低残留的检测要求。
Abstract:A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for the determination of herbicides glufosinate, glyphosate and its metabolite aminomethylphosphonic acid. Pure water was used to extract glufosinate, glyphosate, and aminomethylphosphonic acid from tea, the extract was purified and concentrated with methylene chloride and an anion exchange solid-phase extraction cartridge, eluted with 0.25 mol/L sodium bicarbonate solution, and then derivatization was performed directly with 1% fluorenylmethyloxycarbonyl chloride, the derivatization time was 5 min, and separation was performed by using a reverse phase liquid chromatography column with electrospray positive ion mode and multiple reaction mode (MRM) detection. The mass concentration of glufosinate, glyphosate, aminomethylphosphonic acid in the range of 0-20 μg/L has good linearity, the linear correlation coefficients were more than 0.995, and the limit of quantification was 0.01 mg/kg. In the different tea matrices, the average addition recoveries of 0.01, 0.025, and 0.05 mg/kg were 94.0%-116.0%, and the relative standard deviation of the results was 3.5%-7.1%(n=6). The method is simple, sensitive and accurate, and can meet the requirements for the detection of glufosinate, glyphosate and aminomethanephosphonic acid residues in tea samples.
关键词:高效液相色谱-串联质谱法;草甘膦;草甘膦代谢物氨甲基膦酸;草胺膦;茶叶
Keywords:liquid chromatography-tandem mass spectrometry; glyphosate; glyphosate ammonium metabolites aminomethylphosphonic acid; glufosinate; tea
本文引用格式:
赵春华,左于一菲,孙倩.高效液相色谱-串联质谱法检测茶叶中痕量草胺膦、草甘膦及其代谢物氨甲基膦酸残留[J].化学分析计量,2018,27(5):96-101.
ZHAO C H,ZUOYU Y F,SUN Q. Determination of trace ammonium phosphine,glyphosate and its metabolites residue in tea by LC-MS-MS[J]. Chemical analysis and meterage,2018,27(5):96-101.
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