快速高效液相色谱法同时测定洗发类化妆品中5种去屑剂

Determination of 5 anti-dandruff agents in hair shampoo by high-speed high performance liquid chromatography

目的建立快速高效液相色谱法同时测定去屑产品中水杨酸、吡硫鎓锌、酮康唑、氯咪巴唑和吡罗克酮乙醇胺盐5种去屑剂。方法采用C18柱(50 mm×4.6 nm,2.6μm),流动相为乙腈-甲醇-10 mmol/L磷酸二氢钾(47.5∶7.5∶45,V/V/V,pH值=4.0)含0.5 mmol/L乙二胺四乙酸二钠,流速为2.0 ml/min,柱温为40℃;检测波长为230 nm,标准曲线法定量。结果水杨酸在16.85 mg/L^421.2 mg/L、吡硫鎓锌在9.054 mg/L^226.3 mg/L、酮康唑在18.61 mg/L^465.2 mg/L、氯咪巴唑在18.49 mg/L^462.3 mg/L、吡罗克酮乙醇胺盐在19.96 mg/L^499.0 mg/L时线性关系良好,相关系数均>0.999,平均回收率为100.5%~103.7%,相对标准偏差为1.1%~1.5%,检出限为0.022 mg/L^0.226 mg/L,定量限为0.073 mg/L^0.754 mg/L。测定26批洗发水,有13批检出吡硫鎓锌,4批检出吡罗克酮乙醇胺盐,3批检出水杨酸,2批检出氯咪巴唑,未检出酮康唑。结论本法快速、准确、灵敏,可用于化妆品中5种去屑剂的同时测定。

Objective To develop a method for the determination of 5 anti-dandruff agents including salicylie acid,pyrithione zinc,ketoconazole,climbazole and piroctoneolamine in hair shampoo by high-speed high performance liquid chromatography.Methods C18 column（ 50 mm × 4. 6 nm,2. 6 μm） was used as separation column,and acetonitrile-methanol-10 mmol/L KH2 PO4（ 47. 5∶7. 5∶45,V/V/V,p H = 4. 0） containing 0. 5 mmol/L Na2 EDTA were used as mobile phase,isocratic elution was performed at the flow rate of 2. 0 ml/min,and the detection wavelength was 230 nm,column temperature was 40 ℃. The quantifications were based on standard curves. Results Good linearity was obtained when the concentrations of salicylie acid,pyrithione zinc,ketoconazole,climbazole and piroctoneolamine were within 16. 85 mg/L-421. 2 mg/L,9. 054 mg/L-226. 3 mg/L,18. 61 mg/L-465. 2 mg/L,18. 49 mg/L-462. 3 mg/L,19. 96 mg/L-499. 0 mg/L,respectively,and the correlative coefficients were greater than 0. 999. The average recovery rates of the method were within 100. 5%-103. 7%,with the relative standard deviations（ RSDs） of 1. 1%-1. 5%. The limits of detection of the method were within 0. 022 mg/L-0. 226 mg/L and their limits of quantification were within 0. 073 mg/L-0. 754 mg/L. Among test results of 26 shampoo samples,pyrithione zinc was detected in 13 samples; piroctoneolamine was detected in 4 samples; salicylie acid was detected in 3 samples; climbazole was detected in 2 samples; ketoconazole was not detected. Conclusion The method is fast,sensitive,accurate,and can be applied to the determination of 5 anti-dandruff agents in hair shampoo.