提出了同时测定染发剂中1-萘酚和2-萘酚的高效液相色谱-串联质谱分析方法。染发剂样品经甲醇-水(1+1)混合液萃取,ProElut PLS固相萃取小柱净化,净化液吹氮蒸干后残渣用甲醇溶解并定容为1 mL。此溶液经Agilent ZORBAX SB-C18色谱柱(2.1 mm×150 mm,3.5 μm)分离,用不同体积比混合的乙腈和水梯度洗脱,采用电喷雾负离子模式多反应监测。1-萘酚和2-萘酚的线性范围均为0.05~10.0 mg·L-1,检出限(3S/N)均为0.05 mg·kg-1,测定下限(10S/N)均为0.2 mg·kg-1。方法应用于测定实际样品中上述两化合物。以空白样品作基体加入混合标准溶液做回收试验,测得回收率在82.5%~102%之间,测定值的相对标准偏差(n=10)在6.3%~11%之间。

HPLC-MS/MS was applied to the simultaneous determination of 1-naphthol and 2-naphthol in hair dye. The sample was extracted with a mixture of methanol and water (1+1), and purified on ProElut PLS solid phase extraction column. The eluate was evaporated to dryness by N2-blowing, and the residue was dissolved with and made up to 1 mL of methanol and separated by using Agilent ZORBAX SB-C18 column (2.1 mm×150 mm, 3.5 μm), and mixtures of acetonitrile and water in different ratio as mobile phase for gradient elution. Negative electrospray ionization as well as multiple reaction monitoring mode were used in the detection. Linearity ranges of 1-naphthol and 2-naphthol were found same between 0.05-10.0 mg·L-1, with their detection limits (3S/N) of 0.05 mg·kg-1, and lower limit of determination (10S/N) of 0.2 mg·kg-1. The proposed method was used in the determination of the 2 compounds in substantial samples, and recovery was tested by addition of mixed standard solution to blank samples giving results of recovery in the range of 82.5%-102% with values of RSD′s (n=10) in the range of 6.3%-11%.