一步式提取净化/超高效液相色谱-串联质谱法测定水生蔬菜中矮壮素和灭蝇胺

Determination of chlormequat and cyromazine residues in aquatic vegetables by ultra performance liquid chromatography-tandem mass spectrometry with extraction and purification on one step

中文关键词:  超高效液相色谱-串联质谱法  茭白  慈姑  莲藕  矮壮素  灭蝇胺

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  zizania  arrowhead  lotus root  chlormequat  cyromazine

中文摘要:

      目的 建立一步式提取净化/超高效液相色谱-串联质谱法(ultra performance liquid chromatography- tandem mass spectrometry, UPLC-MS/MS)测定茭白、慈姑和莲藕中矮壮素和灭蝇胺的分析方法。方法 样品经乙腈和盐包[2 g NaCl, 2 g MgSO4, 1.5 g 乙二胺-N-丙基硅烷(primary-secondary amine, PSA)]一步式提取净化, 采用UPLC-MS/MS同时进行检测。结果 矮壮素和灭蝇胺2种农药在0.0025~0.5 mg/L范围内具有良好的线性关系, 且相关系数均大于0.9991。在0.05~0.5 mg/kg范围内, 平均添加回收率为65.4%~83.6%, 相对标准偏差(relative standard deviation, RSD)在1.1%~3.6%之间。结论 该方法操作简单, 准确度高, 适用于水生蔬菜中矮壮素和灭蝇胺2种农药的同时定量测定。

英文摘要:

      Objective To establish a method for the determination of chlormequat and cyromazine in zizania, arrowhead and lotus root by ultra performance liquid chromatography-tandem mass spectrometry (UPLC/MS/MS) with extraction and purification on one step method. Methods The analytes were extracted and purified from sample with acetonitrile and salt packets containing 2 g NaCl, 2 g MgSO4 and 1.5 g ethylenediamine-N- propylsilane(PSA) on one step, then analyzed by UPLC-MS/MS. Results The linear range was from 0.0025? 0.5 mg/L for chlormequat and cyromazine with the good coefficients(r≥0.9991). The recoveries of zizania, arrowhead and lotus root added from 0.05 to 0.5 mg/kg were 65.4%?83.6%, with relative standard deviations(RSD) of 1.1%?3.6%. Conclusion This method is simple, accurate and suitable for the simultaneous quantitative determination of chlormequat and cyromazine in aquatic vegetables.