色谱

色谱 ›› 2012, Vol. 30 ›› Issue (05): 527-532.DOI: 10.3724/SP.J.1123.2011.11049

• 技术与应用 • 上一篇    下一篇

高效液相色谱-串联质谱法同时检测化妆品中6种禁用着色剂

林维宣1*, 孙兴权1, 赵雪蓉1, 徐伟1, 郭桂媛2   

  1. 1. 辽宁出入境检验检疫局技术中心, 辽宁 大连 116001; 2. 大连工业大学生物与食品工程学院, 辽宁 大连 116034
  • 收稿日期:2011-11-25 修回日期:2011-12-30 出版日期:2012-05-28 发布日期:2012-06-07
  • 通讯作者: 林维宣,硕士,研究员,主要从事食品安全检测技术领域的研究. Tel: (0411)82583672, E-mail: dlciqlwx@sina.com.
  • 基金资助:

    国家质量监督检验检疫总局立项课题(课题号: 2009IK-149).

Simultaneous determination of 6 forbidden colorants in cosmetics by high performance liquid chromatography-tandem mass spectrometry

LIN Weixuan1*, SUN Xingquan1, ZHAO Xuerong1, XU Wei1, GUO Guiyuan2   

  1. 1. Liaoning Entry-Exit Inspection and Quarantine Bureau, Dalian 116001, China; 2. School of Biological & Food Engineering, Dalian Polytechnic University, Dalian 116034, China
  • Received:2011-11-25 Revised:2011-12-30 Online:2012-05-28 Published:2012-06-07

PDF

380

被引次数

20

摘要： 建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时测定膏状和粉状化妆品中苏丹红IV、酸性紫49、苏丹蓝2、溶剂红49、碱性紫1和颜料橙5等6种禁用着色剂的检测方法。样品经乙醇-乙腈(3:2, v/v)超声振荡提取20 min、离心净化及氮吹浓缩后,在Luna C18色谱柱(150 mm×2.1 mm, 5 μm)上进行反相液相色谱分离,以甲醇和10 mmol/L乙酸铵溶液为流动相进行梯度洗脱,采用多反应监测(MRM)模式进行质谱测定。根据保留时间及质谱图上特征离子的相对丰度比进行定性,外标法定量。结果表明: 6种着色剂的定量限(信噪比为10计)为0.1～10 μg/kg,回收率为86.67%～98.22%,相对标准偏差(RSD)为4.01%～7.01%。该方法简便、快速、灵敏度高且重现性好,适合于化妆品中禁用着色剂的定性与定量。

关键词: 高效液相色谱-串联质谱, 化妆品, 禁用着色剂

Abstract: A method of high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been established for the simultaneous determination of six forbidden colorants including Sudan IV, Acid Violet 49, Sudan Blue 2, Solvent Red 49, Basic Violet 1 and Pigment Orange 5 in cream and powdery matrix cosmetics. The samples were extracted with ethanol-acetonitrile (3:2, v/v) solution by ultrasonic technique for 20 min, then centrifuged for purification and enriched by nitrogen blowing sequentially. The analytes were isolated on a Luna C18 column (150 mm×2.1 mm, 5 μm) by gradient elution with methanol and 10 mmol/L ammonium acetate as the mobile phases, and detected by MS/MS in the multiple reaction monitoring (MRM) mode. The qualitative analysis was based on the retention time and the relative abundance ratio of the characteristic ions, and the quantitative analysis on calibration curve method. The results showed that the limits of quantification (LOQ, S/N=10) of the six colorants ranged from 0.1 to 10 μg/kg and the average recoveries were from 86.67% to 98.22% with the relative standard deviations (RSDs) from 4.01% to 7.01%. The method is simple and rapid with high sensitivity and good reproducibility, and suitable for the determination of the six forbidden colorants in cosmetics.

Key words: cosmetics, forbidden colorant, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)

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