高效液相色谱法测定氧化型染发产品中47种染发剂

Determination of 47 kinds of dyestuffs in oxidative hair dye by high performance liquid chromatography

建立了测定氧化型染发产品中47种染发剂含量的高效液相色谱分析方法。样品经无水乙醇-10 g/L亚硫酸氢钠水溶液(体积比7∶3)超声提取后,加入2 g/L亚硫酸氢钠水溶液定容至25 mL。采用Shim-pack GIST C18 (4.6 mm×250 mm,5μm)色谱柱分离,分别以乙腈-20 mmol/L磷酸二氢钾溶液(pH7.5)、甲醇-20 mmol/L磷酸二氢钾溶液(pH7.5)为流动相梯度洗脱,流速1.0 mL/min,柱温25℃,检测波长230和280 nm,标准曲线法定量。结果表明,47种染发剂在相应的浓度范围线性关系良好,相关系数均大于0.999,检出限(LOD)为1~35μg/g。在3种加标水平下的平均加标回收率为80.4%~110.7%,相对标准偏差为0.25%~5.08%。与现行标准检验方法相比,该方法增加了15种准用染发剂的测定,具有较高的准确度和精密度,能满足实际检测需求,适用于氧化型染发产品中47种染发剂的测定。

A high performance liquid chromatographic(HPLC) method was developed for the determination of 47 kinds of dyestuffs in oxidative hair dye.The samples were extracted ultrasonically with anhydrous ethanol-10 g/L sodium bisulfite solution(7∶3),and then 2 g/L sodium bisulfite solution was added to a constant volume of 25 m L.If necessary,the extractions were centrifuged at 10 000 r/min for 5 minutes.Chromatographic separation was carried on a Shim-pack GIST C18(4.6 mm×250 mm,5 μm) column by gradient elution.Acetonitrile-20 mmol/L dipotassium hydrogen phosphate(p H7.5) and methanol-20 mmol/L dipotassium hydrogen phosphate(p H7.5) were used as the mobile phase,respectively.The flow rate was 1.0 m L/min and the column temperature was 25 ℃.The analysis of 47 kinds of dyestuffs was performed by HPLC with diode array detector at the wavelength of 230,280 nm,respectively.Quantification analysis was performed by the calibration curve method.The linear ranges of 47 kinds of dyestuffs show good linearity with the correlation coefficients more than 0.999.The limits of detection(LOD) are in the ranges of 1-35 μg/g.The mean recoveries at three different concentration levels are 80.4%-110.7% with the RSDs of 0.25%-5.08%.Compared with the current standard,this method increases the determination of 15 permitted dyes.This method has high accuracy and precision,and can meet the actual detection needs.It is suitable for the determination of 47 kinds of dyestuffs in oxidized hair dyes.