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高效液相色谱法测定化妆品中3种α-羟基酸及其酯

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建立了高效液相色谱法(HPLC)同时测定化妆品中葡糖酸、葡糖酸内酯和乳糖酸的含量,并结合高效液相色谱-串联质谱联用法(HPLC-MS/MS)对结果进行确证.样品经水超声提取,并在氢氧化钠的作用下将葡糖酸、葡糖酸内酯、乳糖酸转化为葡糖酸盐和乳糖酸盐,采用高效液相色谱法,以0.04 mol/L的磷酸氢二铵水溶液和乙腈为流动相进行洗脱,Comixsil HCS(4.6 mm×150 mm,3µm)色谱柱分离,二极管阵列检测器(214 nm)检测,外标法定量.采用高效液相色谱-串联质谱联用法,以0.1%甲酸水溶液和含0.1%甲酸乙腈为流动相进行梯度洗脱,Waters T3-C18(2.1 mm×100 mm,1.8µm)色谱柱分离,电喷雾电离,负离子多反应监测模式定性.结果显示,葡糖酸与乳糖酸在相应线性范围内线性关系良好,相关系数均大于0.999.葡糖酸与葡糖酸内酯的方法检出限为100 μg/g,乳糖酸的方法检出限为500 μg/g.3种化合物4种基质样品加标平均回收率为90.8%~110.1%,相对标准偏差为0.3%~4.4%.该方法操作简便、准确度好、灵敏度高,适用于化妆品中葡糖酸、葡糖酸内酯和乳糖酸的测定.
Determination of 3 kinds of α-hydroxy acids and their esters in cosmetics by high performance liquid chromatography
A method for the simultaneous determination of 3 kinds of α-hydroxy acids and their esters in cosmetics,including gluconic acid,glucolactone and lactose acid,was developed by high performance liquid chromatography(HPLC),and the results were confirmed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The above three substances were extracted ultrasonically with water.The analytes were separated on a Comixsil HCS(4.6 mm×150 mm,3µm)column by elution with 0.04 mol/L diammonium hydrogen phosphate-acetonitrile as mobile phase,and detected at the wavelengths of 214 nm.Quantification analysis was performed by the external standard method.HPLC-MS/MS was used for gradient elution with 0.1%formic acid-acetonitrile containing 0.1%formic acid as mobile phase.The analytes were separated on a Waters T3-C18(2.1 mm×100 mm,1.8µm)column.Qualitative analysis was performed by electronic spray ionization under a negative ion mode with multiple reaction monitoring(MRM).The results indicate that gluconic acid and lactose acid show good linearity in its own concentration range with the correlation coefficient of R2>0.999.The detection limits of gluconic acid and glucolactone are 100 μg/g,and that of lactose acid is 500 μg/g.The average spiked recoveries of these three compounds in 4 cosmetic matrices are all in the range of 90.8%-110.1%,with the RSDs of 0.3%-4.4%.The results indicate that the method is simple,sensitive and accurate,and is suitable for the determination of 3 kinds of α-hydroxy acids and their esters in cosmetics.

cosmeticsgluconic acidglucolactonelactose acidHPLCHPLC-MS/MS

张丽媛、程巧鸳、陈岑、李泽桦、黄柳倩、戚绿叶

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浙江省食品药品检验研究院 国家药监局化妆品动物替代试验技术重点实验室,浙江 杭州 310052

化妆品 葡糖酸 葡糖酸内酯 乳糖酸 高效液相色谱法 高效液相色谱-质谱联用法

2021年《化妆品安全技术规范》制修订项目2022年度浙江省药品监督管理局科技计划

2021036

2024

日用化学工业(中英文)
中国日用化学工业研究院

日用化学工业(中英文)

CSTPCD北大核心
影响因子:0.553
ISSN:1001-1803
年,卷(期):2024.54(1)
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