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日用化学工业（中英文）

日用化学工业 ›› 2015, Vol. 45 ›› Issue (2): 115-120.doi: 10.13218/j.cnki.csdc.2015.02.013

• 分析与检测 • 上一篇    

超高效液相色谱-串联质谱法测定染发剂中2,4,5,6-四氨基嘧啶硫酸盐

欧阳立群, 林钦, 王征, 刘飞, 戴明, 陈言凯, 郑小严   

  1. 福建省产品质量检验研究院 国家加工食品质量监督检验中心,福建 福州 350002
  • 出版日期:2015-02-22 发布日期:2019-04-02
  • 作者简介:欧阳立群(1975-),男,湖南人,高级工程师,博士,电话:(0591)83762015,E-mail:oylq1888@126.com。
  • 基金资助:
    国家质检总局公益性行业科研专项资助项目(2012104013-5)

Determination of 2,4,5,6-tetraaminopyrimidine sulfate in hair dye by ultra high performance liquid chromatography- tandem mass spectrometry

OUYANG Li-qun, LIN Qin, WANG Zheng, LIU Fei, DAI Ming, CHEN Yan-kai, ZHENG Xiao-yan   

  1. National Center of Processed Foods Quality Supervision and Inspection,Fujian Inspection and Research Institute for Product Quality,Fuzhou,Fujian 350002,China
  • Online:2015-02-22 Published:2019-04-02

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摘要： 建立了测定染发剂中2,4,5,6-四氨基嘧啶硫酸盐(TAOS)的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品以体积分数为0.3%的甲酸溶液为提取剂进行超声提取,用Waters BEH-C18色谱柱(100 mm×2.1 mm,1.7 μm)分离,以V(体积分数0.3%的甲酸溶液)∶V(乙腈)=95∶5的混合溶液为流动相进行等度洗脱,在电喷雾正离子模式下采用多反应监测(MRM)模式进行定性和定量分析。结果表明:TAOS在0.020～5.0 mg/L的质量浓度内线性关系良好,线性相关系数大于0.99;检出限(S/N=3)为0.17 mg/kg;定量限(S/N=10)为0.56 mg/kg;回收率为87.5%～96.0%;相对标准偏差(RSD,n=6)为5.7%～8.7%。

关键词: 染发剂, 超高效液相色谱-串联质谱, 2,4,5,6-四氨基嘧啶硫酸盐

Abstract: A method for the determination of 2,4,5,6-tetraaminopyrimidine sulfate (TAOS) in hair dye by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established.Hair dye sample was extracted by 0.3% (volume fraction) formic acid aqueous solution under ultrasonic assistance.The separation was performed with a Waters BEH-C18 column (100 mm×2.1 mm,1.7 μm) and isocratictly eluted by a mixed solution of V(0.3% formic acid aqueous solution)∶V(acetonitrile)=95∶5.Under electrospray positive ion mode,the qualitative and quantitative analysis were performed adopting the multiple reaction monitoring (MRM) mode.The results showed that good linear relationship displays within the range 0.020~5.0 mg/L with the correlation coefficients (R2) more than 0.99.The limit of detection (S/N=3) is 0.17 mg/kg,while the limit of quantification (S/N=10) is 0.56 mg/kg.The average recovery of the spiked samples is in the range of 87.5%~96.0% with the relative standard deviation (RSD,n=6) of 5.7%~8.7%.

Key words: hair dye, ultra high performance liquid chromatography-tandem mass spcetrometry, 2,4,5,6-tetraaminopyrimidine sulfate

中图分类号: 

  • TQ649.4