高效液相色谱法测定化妆品中视黄醇等9种组分

Detection of nine components including retinol in cosmetics by high performance liquid chromatography

建立高效液相色谱法测定化妆品中阿达帕林、维甲酸、异维甲酸、维胺酯、他扎罗汀、视黄醇、视黄醇醋酸酯、视黄醇丙酸酯、视黄醇棕榈酸酯9种成分的含量。以甲醇-异丙醇(体积比55∶45)为提取液,用高效液相色谱仪进行分析,以5 mmol/L乙酸铵(pH值=4.5)-甲醇-异丙醇为流动相,流速为1.0 mL/min,采用色谱柱CAPCELL PAK C18(4.6 mm×250 mm×5μm)分离,在238,325和355 nm检测波长下经HPLC检测,同时对提取剂和提取时间、流动相比例、检测波长等条件进行优化。视黄醇、视黄醇醋酸酯、视黄醇丙酸酯、视黄醇棕榈酸酯、他扎罗汀、异维甲酸、维甲酸、维胺酯和阿达帕林的检出限分别为2.01、0.95、1.72、1.65、0.78、1.23、1.94、5.29和0.22μg/g,定量限分别为6.70、3.17、5.73、5.50、2.60、4.10、6.47、17.63和0.73μg/g,高、中、低不同质量浓度的加标提取回收率在80.56%~112.63%之间,相对标准偏差在0.18%~5.85%之间,在0.12~29.19 mg/L的质量浓度范围内线性关系良好(R2>0.9959)。该方法快速准确,可适用于化妆品中视黄醇类成分含量的测定。

A method for the simultaneous determination of 9 components(adapalin,tretinoin,isotretinoin,viaminate,tazarotene,retinol,retinyl acetate,retinyl propionate,retinol palmitate)in cosmetics by high performance liquid chromatography was established.The effects of extraction solvents on the retinol components were explored,and it is found that when the extraction solvent is methanol-isopropanolas(volume ratio 55∶45),the recovery rate of various retinol components can reach the best level.Meanwhile,to obtain higher sensitivity,the acidic mobile phase methanol-isopropanolassystem was used to separate the retinol components.It is found that when the pH is 4.5 and the concentration is 5 mmol/L,the resolution of the 9 retinol components can achieve the best results.Finally,the 9 retinol components were separated by CAPCELL PAK C18(4.6 mm×250 mm×5μm)column using 5 mmol/L ammonium acetate(pH=4.5)-methanol-isopropanolas as the mobile phase,and qualitative and quantitative analysis was performed by high performance liquid chromatography with DAD detection under the detection wavelength of 238,325 and 355 nm.The flow rate was 1.0 mL/min.The results show that there is a good linear relationship in the range of 0.12-29.19 mg/L between concentration and peak area with R^(2) greater than 0.9959.The limits of detection for adapalin,tretinoin,isotretinoin,viaminate,iazarotene,retinol,retinyl acetate,retinyl propionate,and retinol palmitate are 2.01,0.95,1.72,1.65,0.78,1.23,1.94,5.29 and 0.22μg/g,respectively,and the limits of quantification are 6.70,3.17,5.73,5.50,2.60,4.10,6.47,17.63 and 0.73μg/g,respectively.The average recoveries are from 80.56%to 112.63%,with relative standard deviations in the range of 0.18%to 5.85%.This method has advantages such as simple pretreatment,high sensitivity,rapid and accurate.It is suitable for the simultaneous determination.