色谱

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全自动固相萃取-气相色谱-串联质谱法测定卷烟主流烟气中的3种多环芳烃

边照阳, 唐纲岭*, 陈再根, 庞永强, 姜兴益, 胡清源   

  1. 国家烟草质量监督检验中心, 河南 郑州 450001
  • 收稿日期:2011-04-29 修回日期:2011-05-16 出版日期:2011-10-28 发布日期:2011-10-13
  • 通讯作者: 唐纲岭,硕士,高级工程师,主要从事烟草化学、烟草质量检验研究. Tel: (0371)67672613,

Simultaneous determination of chromium speciation in cosmetics using reversed-phase ion-pair chromatography-inductively coupled plasma mass spectrometry

BIAN Zhaoyang, TANG Gangling*, CHEN Zaigen, PANG Yongqiang, JIANG Xingyi, HU Qingyuan   

  1. China National Tobacco Quality Supervision & Test Center, Zhengzhou 450001, China
  • Received:2011-04-29 Revised:2011-05-16 Online:2011-10-28 Published:2011-10-13

摘要: 以全自动固相萃取技术净化主流烟气萃取液,建立了卷烟主流烟气中苯并[a]芘、苯并[a]蒽和屈艹 3种多环芳烃的气相色谱-串联质谱(GC-MS/MS)测定方法。以吸烟机抽吸卷烟,并以剑桥滤片捕集卷烟主流烟气,然后以含氘代苯并[a]芘内标的环己烷溶液萃取滤片,萃取液经全自动固相萃取仪净化后以GC-MS/MS分离检测。结果表明,苯并[a]芘、苯并[a]蒽和屈艹 的检出限分别为0.05、0.16和0.23 ng/cig,回收率为91.5%~102.1%,相对标准偏差(RSD)均小于5%。该方法的自动化程度高、操作简便、检出限低、重复性好,适用于卷烟主流烟气中苯并[a]芘、苯并[a]蒽 3种多环芳烃释放量的检测。

关键词: 多环芳烃, 卷烟主流烟气, 气相色谱-串联质谱, 全自动固相萃取

Abstract: A method was developed to determine chromium speciation simultaneously in cosmetics using reversed-phase ion-pair chromatography (RP-IPC) with inductively coupled plasma mass spectrometry (ICP-MS). After the extraction with disodium ethylenediaminetetraacetate(EDTA) in a water bath, the sample was separated on an XDB C18 column with the mobile phase of 5% (v/v) methanol-2.0 mmol/L tetrabutylammonium (TBA) (pH 6.0), the flow rate of 1.0 mL/min and the injection volume of 100 μL. The collision cell technology was applied to eliminate the mass interferences of 40Ar12C+and 35Cl16O1H+in the analysis of 52Cr+. The separation was achieved within 5 min. The recoveries of Cr(III) and Cr(VI) ranged from 82.7% to 107.2% with the relative standard deviations (RSDs) less than 5.62%(n=6) with the spiked amounts of 0.01~0.50 μg in different kinds of cosmetic samples. The developed method has the advantages of simplicity, sensitivity and good reproducibility, and can be used for the simultaneous determination of Cr(III) and Cr(VI) in cosmetics.

Key words: cosmetic, inductively coupled plasma mass spectrometry (ICP-MS), speciation, chromium, reversed-phase ion-pair chromatography (RP-IPC)