染发剂中4种p-苯二胺N位取代衍生物的高效液相色谱测定法

Analysis of Four N-Substituted Derivatives of p-Phenylenediamine in Hair Dyes by High Performance Liquid Chromatography

建立了高效液相色谱(HPLC)同时测定染发剂中N,N-双(2-羟乙基)-p-苯二胺硫酸盐(DHPD)、N,N-二甲基-p-苯二胺硫酸盐(DMPD)、N,N-二乙基-p-苯二胺硫酸盐(DEPD)、N-苯基-p-苯二胺盐酸盐(PPD)4种p-苯二胺N位衍生物的方法。采用Agilent Eclipse XDB-C18柱(150 mm×4.6 mm,5μm)为固定相,25 mmol/L磷酸缓冲液(pH 6.0,含0.1%的辛烷磺酸钠)和乙腈为流动相,梯度洗脱,流速1.0 mL/min,柱温25℃,进样量20μL,检测波长250 nm和280 nm。各组分的线性范围为0.1～400 mg/L,相关系数r为0.999 2～0.999 9,检出限为18～108 mg.kg-1,定量下限为42～320 mg.kg-1,RSD<10%,加标回收率为83%～115%。该方法具有简便、快速、准确等特点,基本满足实际样品的分析要求。

A high performance liquid chromatographic （HPLC） method was developed for the deter- mination of N, N-bis （2-hydroxyethyl） -p-phenylenediamine sulfate （ DHPD）, N, N-dimethyl-p-pheny- lenediamine sulfate（DMPD） , N, N-diethyl-p-phenylenediamine sulfate （DEPD） and N-phenyl-p-phe- nylenediamine HCI（PPD）. Dyes were separated on an Eclipse XDB -Cls silica column（ 150 mm × 4. 6 mm, 5 μm, Agilent） using acetonitrile - 25 mmol/L phosphate buffer （ pH = 6. 0, containing 0. 1% 1-heptanesulfonie acid sodium salt） as mobile phase by gradient elution at a flow rate of 1.0 mL/min and a column temperature of 25 ℃. The detection wavelengths were set at 250 nm and 280 nm. Under the optimal conditions, the linear ranges of target componds ranged from 0. 1 mg/L to 400 mg/L, with correlation coefficients of 0. 999 2 -0. 999 9. The detection limits were in the range of 18- 108 mg kg-1 and the quantitation limits were in the range of 42 -320 mg kg-1. The spiked recoveries ranged from 83% to 115% with RSDs less than 10% . The method is simple, rapid and accurate, and is applicable to the analysis of various hair dyes.