QuEChERS/高效液相色谱-串联质谱法同时测定葡萄中18种植物生长调节剂残留  

Simultaneous determination of 18 plant growth regulators in grape by QuEChERS extraction and high performance liquid chromatography-tandem mass spectrometry

作　　者：邱暑婷 林学飞[1] 傅冰梦 金鸿铭 许方鑫 吴淑春[1] 

机构地区：[1]杭州医学院,浙江杭州310053

出　　处：《中国卫生检验杂志》2017年第7期931-936,共6页Chinese Journal of Health Laboratory Technology

基　　金：浙江省大学生科技创新活动计划暨新苗人才计划(2016R436003);浙江省科技厅分析测试科技计划项目(2013C37069)

摘　　要：目的建立一种Qu ECh ERS/高效液相色谱-串联质谱(HPLC-MS/MS)同时测定葡萄中18种植物生长调节剂残留量的分析方法。方法采用含1%乙酸的乙腈提取试样中的植物生长调节剂残留,分散固相萃取净化,以Phenomenex XB-C18(100 mm×2.1 mm,2.6μm)为色谱柱,甲醇和5 mmol/L乙酸铵-0.1%乙酸缓冲溶液为流动相梯度洗脱,在多反应监测(MRM)模式下测定,基质匹配标准溶液外标法定量。结果 18种植物生长调节剂在各自的浓度范围内线性关系良好(r>0.990 0),葡萄中3个添加水平的回收率为71.0%~120.2%,检出限(S/N=3)为0.17μg/kg^2.60μg/kg,定量限(S/N=10)为0.56μg/kg^8.70μg/kg。结论该方法操作简单,具有良好的灵敏度、回收率和重复性。Objective To establish a method for the simultaneous determination of 18 plant growth regulators in grape by Qu EChERS extraction and high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.Methods The plant growth regulator residues were extracted from the samples by acetonitrile（containing 1% acetic acid）,cleaned up with Qu EChERS and then analyzed using HPLC-MS/MS in multiple reaction monitoring（MRM） mode.The chromatographic analysis was carried out on a Phenomenex XB-C18（100 mm × 2.1 mm,2.6 μm） column with methanol and 5 mmol/L ammonium acetate solution（contain 0.1% acetic acid） as the mobile phases in gradient program,and quantified by matrix-matched external standard method.Results The 18 plant growth regulators showed good linearity when the they were in their concentration ranges（r 〉0.990 0）.The recoveries of 18 plant growth regulators in grape were within 71.0%-120.2%.The limits of detection（S/N = 3） were within 0.17 μg/kg-2.60 μg/kg and the limits of quantification（S/N = 10） of the 18 plant growth regulators were within 0.56 μg/kg-8.70 μg/kg.Conclusion The method is simple with high sensitivity,recoveries and good reproducibility.

关 键 词：QUECHERS 高效液相色谱-串联质谱 植物生长调节剂 残留 葡萄 

分 类 号：O657.63[理学—分析化学]