色谱

色谱 ›› 2014, Vol. 32 ›› Issue (6): 653-657.DOI: 10.3724/SP.J.1123.2014.02015

• 技术与应用 • 上一篇    下一篇

气相色谱-三重四极杆质谱法同时测定生脉饮中17种邻苯二甲酸酯类化合物的残留量

张莉1,2, 尚楚翔2, 孙成2   

  1. 1. 江苏省食品药品检验所, 江苏 南京 210008;
    2. 南京大学, 江苏 南京 210093
  • 收稿日期:2014-02-17 修回日期:2014-03-24 出版日期:2014-06-08 发布日期:2014-05-22
  • 通讯作者: 孙成

Simultaneous determination of 17 phthalate esters in Shengmaiyin by gas chromatography-triple quadrupole mass spectrometry

ZHANG Li1,2, SHANG Chuxiang2, SUN Cheng2   

  1. 1. Jiangsu Institute for Food and Drug Control, Nanjing 210008, China;
    2. Nanjing University, Nanjing 210093, China
  • Received:2014-02-17 Revised:2014-03-24 Online:2014-06-08 Published:2014-05-22

PDF

311

被引次数

27

摘要：

建立了气相色谱-三重四极杆质谱（GC-QQQ MS）同时测定生脉饮中17种邻苯二甲酸酯类化合物（PAE）残留量的方法。样品经正己烷振摇提取后进行检测。采用Agilent HP-5MS毛细管色谱柱（30 m×0.25 mm×0.25 μm）在程序升温条件下进行色谱分离；质谱以电子轰击（EI）为电离方式，采用多反应监测（MRM）模式进行监测。实验结果表明：17种PAE在0.5~20 mg/L范围内呈线性关系，r均大于0.99；平均加标回收率除邻苯二甲酸二甲酯（DMP）为51.9%、邻苯二甲酸二乙酯（DEP）为77.2%外，其余15种为91.8%~117.2%，RSD（n=6）为0.5%~5.4%。该方法操作简便，准确可靠，灵敏度高，专属性强，可用于生脉饮中邻苯二甲酸酯类化合物残留量的检测，以控制生脉饮的用药安全。

关键词: 邻苯二甲酸酯, 气相色谱-质谱法, 生脉饮, 塑化剂, 中药口服液

Abstract:

Phthalate esters (PAEs) are commonly used for plastic products as plasticizer. Once taken in by human, PAEs will cause diseases, such as endocrine disorders, cancer, etc. Shengmaiyin is a kind of Chinese medicine oral fluid whose packaging materials may include phthalate esters. If the phthalate esters migrated into the solution, it would lead to serious problem on the safety of drugs. In this study, a method of gas chromatography coupled to triple quadrupole mass spectrometry (GC-QQQ-MS) was developed for the simultaneous determination of 17 phthalate esters in Shengmaiyin samples. The samples were extracted with n-hexane by liquid-liquid extraction method before analysis. The separation was performed on an HP-5MS capillary column (30 m×0.25 mm×0.25 μm) with temperature programming. The MS/MS detection was performed under electron impact source (EI) in multi-reaction monitoring (MRM) mode. The good linear relationships were obtained in the range of 0.5-20 mg/L for all the target analytes. The average recoveries of the 15 PAEs were in the range of 91.8%-117.2%, except dimethyl phthalate and diethyl phthalate which were about 51.9% and 77.2%, respectively, and all the RSDs were in the range of 0.5%-5.4% (n=6). The limits of detection ranged from 0.04 to 16.76 μg/L. The developed GC-MS method is simple, accurate, sensitive, proprietary, and can be applied in the detection of the phthalate ester residues in Shengmaiyin.

Key words: Chinese medicine oral fluid, gas chromatography-mass spectrometry (GC-MS), phthalate esters, plasticizer, Shengmaiyin

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