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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
Determination of 2,4,5,6-tetraaminopyrimidine sulfate in hair dye by ultra high performance liquid chromatography- tandem mass spectrometry
欧阳立群, 林钦, 王征, 刘飞, 戴明, 陈言凯, 郑小严
2015 (2):
115-120.
doi: 10.13218/j.cnki.csdc.2015.02.013
摘要
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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%。
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%.
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