马春艳, 路惬楠, 段琼, 胡伟杰, 封淑华, 刘雪莉. 保健酒中酞酸酯污染物的气相色谱-三重四极杆质谱法测定[J]. 分析测试技术与仪器, 2018, 24(1): 23-27. DOI: 10.16495/j.1006-3757.2018.01.004
引用本文: 马春艳, 路惬楠, 段琼, 胡伟杰, 封淑华, 刘雪莉. 保健酒中酞酸酯污染物的气相色谱-三重四极杆质谱法测定[J]. 分析测试技术与仪器, 2018, 24(1): 23-27. DOI: 10.16495/j.1006-3757.2018.01.004
MA Chun-yan, LU Qie-nan, DUAN Qiong, HU Wei-jie, FENG Shu-hua, LIU Xue-li. Determination of Phthalates Contaminants in Health Care Wine by Gas Chromatography-QQQ Mass Spectrometry[J]. Analysis and Testing Technology and Instruments, 2018, 24(1): 23-27. DOI: 10.16495/j.1006-3757.2018.01.004
Citation: MA Chun-yan, LU Qie-nan, DUAN Qiong, HU Wei-jie, FENG Shu-hua, LIU Xue-li. Determination of Phthalates Contaminants in Health Care Wine by Gas Chromatography-QQQ Mass Spectrometry[J]. Analysis and Testing Technology and Instruments, 2018, 24(1): 23-27. DOI: 10.16495/j.1006-3757.2018.01.004

保健酒中酞酸酯污染物的气相色谱-三重四极杆质谱法测定

Determination of Phthalates Contaminants in Health Care Wine by Gas Chromatography-QQQ Mass Spectrometry

  • 摘要: 建立了气相色谱-三重四极杆质谱(GC-MS/MS)联用法检测保健酒中的16种酞酸酯的方法.对保健酒中酞酸酯的前处理方法进行了考察和优化,确立了提取方式为沸水浴加热去除乙醇、提取溶剂为正己烷.采用时间选择反应扫描模式(T-SRM)定量.色谱柱为TG-5MS石英毛细管柱(30 m×0.25 mm×0.25 μm),程序升温(初始柱温为60℃,保持1 min,以20℃/min升至220℃,保持1 min;以5℃/min升至280℃,保持4 min),不分流.结果表明16种酞酸酯在相应范围内线性关性良好(R2均高于0.995),平均回收率在84.0%~112.8%,RSD均低于7%(n=6).采用方法对6批保健酒中酞酸酯进行测定,结果表明方法具有灵敏、简单快速、结果准确可靠等优点,GC-MS/MS联用法可满足保健酒中酞酸酯的定性分析和含量测定.

     

    Abstract: A method for the determination of 16 phthalates in the health care wine by gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS) was developed. Pretreatment methods of phthalate esters in health care wine were studied and optimized. An extraction method to remove ethanol on a boiling water bath was established, using n-hexane as the extractant. Quantitative analysis was performed on the time selective reaction scanning mode (T-SRM). The chromatographic column used was a TG-5MS quartz capillary column (30 m×0.25 mm×0.25 μm), the programmed temperature (initial column temperature was 60℃, kept for 1 min, and raised to 220℃ at 20℃/min, kept for 1 min, then kept at 5℃/min to 280℃, kept for 4 min), without shunting. The results showed that the 16 phthalates had an effective internal correlation (R2 > 0.995). The average recovery was 84.0%~112.8%, and the RSD was less than 7% (n=6). 6 PAEs in health care wine were determined by this method. The results showed that the method is sensitive, simple and rapid, accurate and reliable. The GC-MS/MS method can satisfy the qualitative analysis and quantitative determination of the phthalates in health care wine.

     

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