化妆品中α-熊果苷等4种原料的含量测定及方法确认

Determination and method confirmation ofα-arbutin and other 4 raw materials in cosmetics

目的:采用高效液相色谱-荧光检测法(HPLC-FLD)同时测定美白类化妆品中α-熊果苷、β-熊果苷、氢醌和苯酚等4种原料的含量,分析检测方法的准确性。方法:样品用甲醇提取,SHIMADZU Shim-pack GIST C18柱(250 mm×4.6 mm×5μm)分离,甲醇-水流动相梯度洗脱,流速0.5 mL/min,进样量5μL。结果:α-熊果苷、β-熊果苷、氢醌和苯酚4种原料浓度分别为0.25~20、0.25~20、0.025~2和0.05~4 mg/L范围内线性良好(相关系数r>0.999);检出限S/N>3,定量限S/N>10;在液态水基、膏霜乳液、凝胶、面膜和粉类化妆品均无4种原料检出情况下,进行空白基质加标,方法回收率范围为95.4%~103.8%;日内相对标准偏差RSD范围为0.2%~1.8%,日间相对标准偏差RSD范围为0.6%~2.7%(n=6);30批美白类化妆品中,5批检出α-熊果苷,含量范围在80~380μg/g;7批检出β-熊果苷,含量范围在90~546μg/g。结论:《化妆品安全技术规范》(2015年版)第四章8.2化妆品中α-熊果苷等4种原料检验方法简便、快速、准确、灵敏,可用于美白类化妆品中α-熊果苷、β-熊果苷、氢醌和苯酚等4种原料的同时定量测定。

Objective:The high performance liquid chromatography-fluorescence detection(HPLC-FLD)was used to determine the contents ofα-arbutin,β-arbutin,hydroquinone,and phenol in whitening cosmetics,and the accuracy of the detection method was analyzed.Methods:The samples were extracted with methanol,separated by SHIMADZU Shimpack GIST C18 column(250 mm×4.6 mm×5μm),eluted by methanol-water mobile phase gradient at the flow rate of 0.5 mL/min,and the sample size was 5μL.Results:The concentrations ofα-arbutin,β-arbutin,hydroquinone,and phenol were in the ranges of 0.25~20 mg/L,0.25~20 mg/L,0.025~2 mg/L,and 0.05~4 mg/L respectively(correlation coefficient r>0.999),with detection limit>3 and quantification limit>10.When no raw material was detected in liquid water,cream,lotion,gel,mask,or powder cosmetics,the blank matrix was added,and the recovery range was 95.4%~103.8%.Intra-day RSD ranged from 0.2%to 1.8%,and intra-day RSD ranged from 0.6%to 2.7%(n=6).Among 30 batches of whitening cosmetics,α-arbutin was detected in 5 batches with the content ranging from 80 to 380μg/g.β-arbutin was detected in 7 batches with the content ranging from 90 to 546μg/g.Conclusion:The method for the determination ofα-arbutin and other 3 raw materials in the Clause 8.2 of Chapter 4 of the Technical Code for Safety of Cosmetics(2015 edition)is simple,rapid,accurate,and sensitive,and can be used for the simultaneous quantitative determination ofα-arbutin,β-arbutin,hydroquinone,and phenol in whitening cosmetics.