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作 者:刘向红 林小娟 龙慧端 邓鸣 谢东 许有诚 张科明 LIU Xianghong;LIN Xiaojuan;LONG Huiduan;DENG Ming;XIE Dong;XU Youcheng;ZHANG Keming(Guangxi Institute for Food and Drug Control,Nanning 530021,Guangxi,China)
出 处:《香料香精化妆品》2023年第2期40-45,64,共7页Flavour Fragrance Cosmetics
基 金:广西药品监督管理局2021年直属单位药品安全科研项目计划(编号2021-06)。
摘 要:本文建立了分散固相微萃取-氨基酸自动分析仪同时测定化妆品中20种游离氨基酸(包括常规18种氨基酸以及牛磺酸、5-氨基乙酰丙酸等非蛋白氨基酸)的方法。将样品加入硫酸铝等分散介质和样品稀释液,涡旋、分散、超声提取后测定,采用0.04mol/L柠檬酸钠缓冲液(pH 3.45)和0.07mol/L柠檬酸钠缓冲液(pH 10.85)为流动相梯度洗脱,经LCA K06/Na磺基强酸型阳离子交换树脂色谱柱(150mm×4.6mm×5μm)分离,茚三酮柱后衍生,检测波长440 nm和570 nm。该方法中20种氨基酸色谱分离良好,线性相关系数r>0.999,检出限0.1~3.7mg/kg,加标回收率80.7%~115%,相对标准偏差为0.1%~3.9%。该方法操作简便、重复性良好、结果准确可靠,适用于化妆品中20种游离氨基酸成分的测定。A method based on automatic amino acid analyzer coupled with dispersive micro solid-phase extraction was developed for the simultaneous determination of 20 free amino acids,including 18 conventional amino acids and non-protein amino acids such as taurine(Tau)and 5-aminolevulinic acid(5-ALA).The cosmetic products were ultrasonically extracted by sample dilution,after adding aluminum sulfate and other dispersion media.Gradient elution was carried out with 0.04 mol/L sodium citrate buffer(pH 3.45)and 0.07 mol/L sodium citrate buffer(pH 10.85)as the mobile phase.Then the amino acids were separated on an LCA K06/Na column(150 mm×4.6 mm×5μm),analyzed by the post-column which was derivatized with ninhydrin,and detected at the wavelengths of 440 nm and 570 nm.The developed method showed good linearity,with the correlation coefficients greater than 0.999,and the limits of detection of the 20 amino acids were 0.1-3.7 mg/kg.The average recoveries ranged from 80.7%to 115%,and the relative standard deviations were in the range of 0.1%to 3.9%.This method is simple, reproducible, accurate, reliable and suitable for the determination of the 20 free amino acids in cosmetic products.
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