摘要
[目的]建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS)测定人参中17种有机氯类农药残留量。[方法]对不同产地人参样品利用丙酮水溶液超声进行提取,加入二氯甲烷及氯化钠,并应用盐析原理使有机相与水相较好分层,使农药由水相进入有机相,取出一部分有机相浓缩净化,提取液采用GC-MS,经以键合交联5%苯基甲基硅氧烷为固定液(HP-5)的毛细管柱(30 m×0.32 mm×0.25μm),初始温度60℃,保持0.3 min,以60℃/min升至170℃,再以10℃/min升至220℃,保持10 min,再以1℃/min升至240℃,15℃/min升至280℃,保持5 min的程序升温过程进行检测分析。[结果]17种有机氯类农药在1.00~106.00 ng/mL范围内线性关系良好,检测限为0.005~0.020 mg/kg,3个水平的添加回收率在75%~120%。[结论]该方法简单、灵敏、稳定、可靠,可用于测定人参中17种有机氯类农药残留量。
[Objective]The research aimed to establish gas chromatography-tandem mass spectrometry(GC-MS)for the determination of 17 organochlorine pesticide residues in ginseng.[Method]The ginseng samples from different producing areas were extracted by ultrasonication with acetone solution,and dichloromethane and sodium chloride were added.The principle of salting out was used to separate the organic phase and the aqueous phase,and the pesticide was separated from the aqueous phase into the organic phase.The phase was concentrated and purified,and the extract was subjected to GC-MS,and a capillary column(30 m×0.32 mm×0.25μm)which was bonded and crosslinked with 5%phenylmethylsiloxane as a fixing solution(HP-5),and an initial temperature of 60℃,hold for 0.3 minutes,increase to 170℃at 60℃/min,then increase to 220℃at 10℃/min for 10 minutes,then rise to 240℃at 1℃/min,raised to 280℃at 15℃/min,and the temperature-programming process was carried out for 5 minutes for detection and analysis.[Result]The linearity of 17 organochlorine pesticides in the range of 1.00-106.00 ng/mL was good,the detection limit was 0.005-0.020 mg/kg,and the recovery rate of the three levels was 75%-120%.[Conclusion]The method is simple,sensitive,stable and reliable,and can be used for determining 17 organochlorine pesticide residues in ginseng.
作者
丁慧
钱勇
DING Hui;QIAN Yong(.Shanghai Bainianshidande Testing Technology Co.,Ltd.,Shanghai 201314;Shanghai Shidande Standard Technology Service Co.,Ltd.,Shanghai 201314)
出处
《安徽农业科学》
CAS
2020年第3期197-199,214,共4页
Journal of Anhui Agricultural Sciences
基金
上海市科委科研计划项目(18DZ2291600)
