高效液相色谱-质谱法同时测定染发剂中33种禁限用染料

Simultaneous determination of 33 kinds of banned and/or restricted component in hair dyes by high performance liquid chromatography-mass spectrometry

建立了高效液相色谱-质谱（HPLC-MS/MS）同时测定染发剂中33种禁限用染料的方法。样品用甲醇和2 g/L抗坏血酸水溶液的混合溶液溶解,正己烷净化,以5 mmol/L的乙酸铵水溶液和乙腈为流动相进行梯度洗脱,经Agilent ZORBAX Extend C18柱（2.1 mm×100 mm,1.8μm）分离。在电喷雾离子模式下,采用多重反应监测模式（MRM）进行定性和定量分析。33种染料在相应的质量浓度范围内线性关系良好,线性相关系数均大于0.99,检出限为0.01~29.5 mg/kg,回收率为71%~115%。

A high performance liquid chromatography- mass spectrometry（ HPLC- MS / MS） method was established for simultaneous determination of 33 kinds of banned and / or restricted component in hair dyes.After extracted by mixed solution with methanol and 2 g / L ascorbic acid aqueous solution,purified by n-hexane,the samples were analyzed by HPLC- MS / MS. The separation was performed on an Agilent ZORBAX Extend C18column（ 2. 1 mm × 100 mm,1. 8 μm） and gradient eluted with aqueous solution of 5 mmol / L ammonium acetate and acetonitrile. The electro spray ionization source in positive and negative ion mode was used for qualitative and quantitative analysis of the 33 components under the multiple reaction monitoring mode（ MRM）. The results show good linear relationships with all correlation coefficients higher than 0. 99. The limits of detection for the 33 components are in the range of 0. 01- 29. 5 mg / kg. The average spiked recoveries of the 33 components are in the range of 71%- 115%.