摘要
目的建立气相色谱-质谱联用法(GC-MS)同时测定人参中五氯苯胺和腐霉利的方法。方法称取一定量的样品,加入乙腈超声提取,离心后取上清液,经氮吹仪浓缩至干后,准确加入1.0 ml的乙腈进行复溶,采用选择离子监测(SIM)模式,通过气相色谱-质谱联用仪进行检测,以外标法定量。结果五氯苯胺和腐霉利的质量浓度为0.005μg/ml^0.5μg/ml时,线性关系良好,相关系数(r)分别为0.999 9、0.999 8,检出限分别为1.0μg/kg、1.2μg/kg。在低、中、高(5.0μg/kg、10.0μg/kg、20μg/kg)3种浓度水平下,方法的回收率为90.5%~109.1%,相对标准偏差(RSD)均<3.0%。结论该方法具有样品前处理操作简单、快速、准确性好、灵敏度高等特点,可用于人参中的五氯苯胺和腐霉利残留的快速检测。
Objective To establish a method for the determination of pentachloroaniline and procymidone residues in ginseng by gas chromatography- mass spectrometry（ GC- MS）. Methods Sample was quantified for ultrasonical extraction with acetonitrile. Centrifuged the supernatant was obtained,and then dried- up and concentrated with pressured gas blowing concentrators.Then the residues were redissolved with 1. 0 ml acetonitrile and determined by GC- MS,which were identified in selected ion monitoring（ SIM） mode. The target compounds were quantified by external standard method. Results The calibration curves for pentachloroaniline and procymidone were linear in the range of 0. 005 μg / m L- 0. 5 μg / m L,and the relative coefficients（ r）were 0. 999 9 and 0. 999 8,respectively,with the detection limit of 1. 0 μg / kg and 1. 2 μg / kg. The average recoveries ranged from 90. 5% to 109. 1% at three concentration levels of 5. 0 μg / kg,10. 0 μg / kg and 20 μg / kg,with the relative standard deviations（ RSD） lower than 3. 0%. Conclusion The method has advantages of rapid determination,good accuracy and high sensitivity,and can be used for rapid detection of pentachloroaniline and procymidone in ginseng.
出处
《中国卫生检验杂志》
CAS
2015年第21期3624-3625,3628,共3页
Chinese Journal of Health Laboratory Technology
关键词
五氯苯胺
腐霉利
人参
气相色谱-质谱联用法
Pentachloroaniline
Procymidone
Ginseng
Gas chromatography-mass spectrometry
