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目的建立高效液相色谱(HPLC)-二极管阵列检测器(DAD)法测定染发剂中20种染料成分的含量,对《化妆品卫生规范》中的氧化型染料的HPLC检测方法进行改进和补充。方法样品经乙醇-水超声提取,过滤后进样检测。色谱柱:Agilent Zorbax Bonus-RP(4.6mm×250mm,5μm);流动相:A相为乙腈,B相为4mmol/L磷酸盐缓冲液(pH 6.0,含0.1%的辛烷磺酸钠离子对试剂),梯度洗脱:0~24min,10%A;24~26min,10%~40%A;26~45min,40%A;45~47min,40%~80%A;47~52min,保持80%A不变;流速1mL/min;柱温15℃,使用DAD进行检测,检测波长为280nm,进样量5μL。结果各染料成分在50min内基线分离。在10.0~500.0mg/L浓度范围内,线性关系良好,相关系数均高于0.999。日内及日间精密度均小于4%,加样回收率为81.90%~119.88%。结论该方法简便、快速、准确,适于氧化型染发剂中染料成分的检测。
OBJECTIVE To establish a method for the determination of 20 kinds of dye components in hair dye by high performance liquid chromatography (HPLC) with diode array detector (DAD) and to improve and supplement HPLC detection method of oxidative dye in Cosmetic Hygienic Standard. Methods Samples were ethanol - water ultrasonic extraction, filtered and injected. Column: Agilent Zorbax Bonus-RP (4.6 mm × 250 mm, 5 μm); Mobile phase: Phase A was acetonitrile and phase B was 4 mmol / L phosphate buffer pH 6.0 with 0.1% sodium octane sulfonate ion pair Reagents), gradient elution: 0-24 min, 10% A; 24-26 min, 10-40% A; 26-45 min, 40% A; 45-47 min, 40-80% A; 80% A constant; flow rate 1mL / min; column temperature 15 ℃, using DAD for detection, the detection wavelength was 280nm, injection volume 5μL. The results of the dye composition within 50min baseline separation. In the concentration range of 10.0 ~ 500.0mg / L, the linear relationship was good, the correlation coefficient was higher than 0.999. The intra-day and inter-day precision were less than 4%, the recovery rate was 81.90% ~ 119.88%. Conclusion The method is simple, rapid and accurate and suitable for the detection of dye components in oxidative hair dyes.