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

摘要

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(pH6.0,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0.9992～0.9999,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 HCl(PPD). Dyes were separated on an Eclipse XDB - C18 silica column(150 mm x 4.6 mm, 5 u^m, Agilent) using acetonitrile -25 mmol/L phosphate buffer(pH =6.0, containing 0. 1% 1 -heptanesulfonic acid sodium salt) as mobile phase by gradient elution at a flow rate of 1. 0 mL/min and a column temperature of 25 X.. 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 quantisation 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.