色谱

色谱 ›› 2016, Vol. 34 ›› Issue (3): 340-345.DOI: 10.3724/SP.J.1123.2015.10034

• 研究论文 • 上一篇    下一篇

气相色谱-负化学电离源-飞行时间质谱测定烟草中有机氯农药残留

司晓喜1, 陆舍铭1, 刘志华1, 朱丽2, 刘春波1, 张凤梅1, 何沛1, 朱瑞芝1   

  1. 1. 云南省烟草化学重点实验室, 云南中烟工业有限责任公司技术中心, 云南 昆明 650231;
    2. 云南中烟物资(集团)有限责任公司, 云南 昆明 650031
  • 收稿日期:2015-10-23 出版日期:2016-03-08 发布日期:2012-09-28
  • 通讯作者: 朱瑞芝
  • 基金资助:

    云南中烟工业有限责任公司技术中心科技项目(S-6013047);红塔烟草(集团)有限责任公司科技项目(K-10006.14).

Determination of organochlorine pesticide residues in tobacco by gas chromatography-negative chemical ionization-time of flight mass spectrometry

SI Xiaoxi1, LU Sheming1, LIU Zhihua1, ZHU Li2, LIU Chunbo1, ZHANG Fengmei1, HE Pei1, ZHU Ruizhi1   

  1. 1. Key Laboratory of Tobacco Chemistry of Yunnan, R & D Center of China Tobacco Yunnan Industrial Co., Ltd., Kunming 650231, China;
    2. Yunnan Tobacco Materials (Group) Co., Ltd., Kunming 650031, China
  • Received:2015-10-23 Online:2016-03-08 Published:2012-09-28
  • Supported by:

    Science & Technology Project of Research & Development Center of China Tobacco Yunnan Industrial Co., Ltd. (No. S-6013047); Science & Technology Project of Hongta Tobacco (Group) Co., Ltd. (No. K-10006.14).

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摘要：

采用QuEChERS前处理方法,建立了气相色谱-负化学电离源-飞行时间质谱(GC-NCI-TOF-MS)检测烟草中10种有机氯农药残留的分析方法。样品采用乙酸乙酯-正己烷(1 : 1, v/v)溶液提取,提取液经N-丙基乙二胺(PSA)、无水硫酸镁分散固相萃取净化,用GC-NCI-TOF-MS检测分析。根据有机氯化合物特征离子的精确质量数、同位素离子峰簇、碎片离子丰度比和保留时间对目标物定性鉴定,外标法定量。10种有机氯农药的线性关系良好,相关系数 (r2)均大于0.997;相对标准偏差小于6.5%;检出限为0.04~0.80 μ g/kg;加标回收率为77.2%~93.0%。该方法简单快速、灵敏度高、准确性好,适用于烟草中有机氯农药残留的定性分析和定量检测。

关键词: QuEChERS, 气相色谱-负化学电离源-飞行时间质谱, 烟草, 有机氯农药

Abstract:

A method was developed for the determination of 10 organochlorine pesticide (OCP) residues in tobacco by gas chromatography-negative chemical ionization-time of flight mass spectrometry (GC-NCI-TOF-MS) coupled with QuEChERS method. The extraction and purification procedures for tobacco samples, the chromatographic conditions and TOF-MS conditions of the analytes were critically examined. Tobacco samples were extracted with ethyl acetate-hexane (1 : 1, v/v) and cleaned up by primary secondary amine (PSA) and MgSO4, then detected by GC-NCI-TOF-MS. Accurate mass analysis, isotopic peak clusters, fragment ion abundance ratio and retention time were employed to qualitative identification and external standard method was used for quantitative determination. The results indicated that the correlation coefficients (r2) were better than 0.997, and the relative standard deviations (RSDs) were less than 6.5%. The limits of detection and the limits of quantification were 0.04 to 0.80 μ g/kg and 0.13 to 2.64 μ g/kg, respectively. The recoveries of the 10 organochlorine pesticides at three spiked levels ranged from 77.2% to 93.0%. It was proved that the method is simple, rapid, with high accuracy and high sensitive. It is appropriate for the detection and determination of organochlorinepesticide residues in tobacco samples.

Key words: gas chromatography-negative chemical ionization-time of flight mass spectrometry (GC-NCI-TOF-MS), organochlorine pesticide (OCP), QuEChERS, tobacco

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