固相萃取-气相色谱-质谱联用法检测啤酒中酰胺类除草剂及其中间体物质

Simultaneous detection of amide herbicides and their intermediates in beer by solid-phase extraction coupled with gas chromatography-mass spectrometry

中文关键词:  酰胺类除草剂  芳香胺  气相色谱-质谱联用法  固相萃取  啤酒

英文关键词:amide herbicides  aromatic amines  gas chromatography-mass spectrometry  solid phase extraction  beer

中文摘要:

      目的 建立固相萃取-气相色谱-质谱联用法(gas chromatography-mass spectrometry, GC-MS)建立同时测定啤酒中8种酰胺类除草剂和2种芳香胺的分析方法。方法 稀释过的样品, 经活化后的C18固相萃取小柱吸附, 用乙腈-甲苯(3:1, V:V)的混合溶液洗脱, DB-5 MS石英毛细管柱分离以及GC-MS的定性和定量分析。 结果 在线性范围0.1~20 μg/L内, 本方法的线性关系良好, 检出限为2.37~10.28 ng/L。在3个加标浓度(0.1、1和10 μg/L)下, 回收率在92.1%~113.9%之间, 相对标准偏差(relative standard deviation, RSD)在2.6%~5.4%之间。将所建立的方法对其他3种啤酒进行了检验, 未检出10种目标物。结论 本研究建立的方法操作简单、回收率高、准确度高, 可以应用到检测啤酒中酰胺类除草剂及其中间体物质。

英文摘要:

      Objective To establish a method for simultaneous determination of 8 kinds of amide herbicides and 2 kinds of aromatic amines in beer by solid-phase extraction (SPE) combined with gas chromatography-mass spectrometry (GC-MS). Methods The diluted samples were absorbed by activated C18 solid-phase extraction column. Then they were eluted by a mixed solution of acetonitrile-toluene (3:1, V:V), and separated by DB-5 MS quartz capillary column. GC-MS was used for qualitative and quantitative analysis. Results In the range of 0.1- 20 g/L, this method had good linear relationships and the limits of detection were 2.37-10.28 ng/L. At the spiked levels of 0.1, 1 and 10 μg/L, the average recoveries were 92.1%-113.9%, and relative standard deviations (RSDs) were 2.6%-5.4%. The developed method had been applied to detect another three brands of beer, but none of the targets had been detected. Conclusion The established method is simple, with high recovery and high accuracy, which can be applied to detect amide herbicides and their intermediates in beer.