色谱

色谱 ›› 2013, Vol. 31 ›› Issue (11): 1040-1045.DOI: 10.3724/SP.J.1123.2013.05032

• 研究论文 • 上一篇    下一篇

固相萃取-超高效液相色谱-串联质谱法测定人指甲中的三氯生和三氯卡班

石莹1,2, 张晶1,2, 卢丽彬1,2, 邵兵1,2,3   

  1. 1. 首都医科大学公共卫生学院, 北京 100069;
    2. 北京市疾病预防控制中心, 食物中毒诊断溯源技术北京市重点实验室, 北京 100013;
    3. 北京市预防医学研究中心, 北京 100013
  • 收稿日期:2013-05-20 修回日期:2013-06-17 出版日期:2013-11-28 发布日期:2013-12-05
  • 通讯作者: 邵兵
  • 基金资助:

    国家自然科学基金项目(21177014);北京市卫生系统高层次卫生技术人才培养计划项目.

Determination of triclosan and triclocarban in human nails by solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry

SHI Ying1,2, ZHANG Jing1,2, LU Libin1,2, SHAO Bing1,2,3   

  1. 1. School of Public Health, Capital Medical University, Beijing 100069, China;
    2. Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Centers for Disease Prevention and Control, Beijing 100013, China;
    3. Beijing Centers for Preventive Medical Research, Beijing 100013, China
  • Received:2013-05-20 Revised:2013-06-17 Online:2013-11-28 Published:2013-12-05

PDF

239

被引次数

8

摘要：

建立了人指甲中三氯生和三氯卡班的固相萃取结合超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。指甲样品经氢氧化钠消化,C18柱富集净化后,通过Waters ACQUITYTM UPLC HSS T3色谱柱(100 mm×2.1 mm, 1.8 μm) 分离,以甲醇和水为流动相进行梯度洗脱,采用三重四极杆串联质谱仪负离子模式进行检测,同位素内标法定量。三氯生和三氯卡班分别在0.5~500.0 μg/kg和0.1~100.0 μg/kg范围内线性关系良好,相关系数(r2)均为0.999,方法定量限分别为2.0 μg/kg和0.2 μg/kg。3个水平的平均加标回收率为95.9%~110.2%,相对标准偏差为0.6%~9.7%(n=6)。本方法具有良好的灵敏度、回收率和重复性,适合指甲中痕量目标污染物的测定。利用该方法分析了60份实际样品,目标物的检出率为100%,三氯生和三氯卡班的含量范围分别为

关键词: 超高效液相色谱-串联质谱, 固相萃取, 三氯卡班, 三氯生, 指甲

Abstract:

An analytical method was developed to simultaneously detect triclosan (TCS) and triclocarban (TCC) in human nails using solid phase extraction (SPE) with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Nail clippings were digested by sodium hydroxide, and then concentrated and purified with C18 cartridges. Chromatographic separation was performed on a Waters ACQUITYTM UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm) with gradient elution using methanol and water at a flow rate of 0.3 mL/min. The target compounds were determined by triple quadrupole mass spectrometer operated in the negative ion mode and quantified by isotopic-dilution technique. The satisfactory linearities (r2=0.999) was obtained over the ranges of 0.5-500.0 μg/kg for TCS and 0.1-100.0 μg/kg for TCC, with the limits of quantification (LOQs) of 2.0 μg/kg for TCS and 0.2 μg/kg for TCC. The average recoveries of the two target compounds (spiked at three concentration levels) ranged from 95.9% to 110.2%, with the relative standard deviations (RSDs) between 0.6% and 9.7% (n=6). This method can be applied in rapid detection of target contaminants in nails due to its high sensitivity, high recovery and good reproducibility. Sixty collected human nail samples were analyzed by means of the developed method. TCS and TCC were detected in all samples with content ranges of

Key words: nail, solid phase extraction (SPE), triclocarban, triclosan, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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