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

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,1.7μm）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） of5. 7% - 8. 7%.