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作 者:张江维[1] 张弦[1] 谭杰[1] 梁柱业 关漪莲 ZHANG Jiangwei;ZHANG Xian;TAN Jie;LIANG Zhuye;GUAN Yilian(Guangdong Institute for Drug Control,Guangzhou 510663,China)
机构地区:[1]广东省药品检验所,广州510663
出 处:《化学分析计量》2024年第5期12-18,共7页Chemical Analysis And Meterage
基 金:2022年广东省药品监督管理局科技创新资助项目(2022TDZ07)。
摘 要:建立高效液相色谱法测定化妆品中19种非甾体抗炎药含量。化妆品样品经体积比为1∶1的乙腈-乙酸铵溶液超声提取,用C_(18)色谱柱(250 mm×4.6 mm,5μm)分离,以不同体积比的乙腈-乙酸铵溶液为流动相梯度洗脱,采用二极管阵列检测器检测。布洛芬的检测波长为230 nm,醋氯芬酸、双氯芬酸钠检测波长为278 nm,其余16种非甾体的检测波长均为245 nm。19种非甾体的质量浓度在5~200μg/mL范围内与其对应的色谱峰面积线性关系良好,相关系数均大于0.999 5,检出限为0.2~8 mg/kg。空白样品的水剂和凝胶基质的加标平均回收率分别为93.1%~110.9%和91.3%~108.1%,测定结果的相对标准偏差分别为0.2%~3.5%和0.6%~4.2%(n=6)。该方法适用于化妆品中19种非甾体抗炎药的测定。A method for the determination of 19 non-steroidal anti-inflammatory drugs(NSAIDs)in cosmetics by high performance liquid chromatography(HPLC)was stablished.The samples were extractedby ultrasound with volume ratio 1∶1 acetonitrile-ammonium acetate solution,separated by C18 column,with different volume ratios of acetonitrile-ammoniumacetate solutionas mobile phase under gradient elution,and detected by diode-array-detector.The detection wavelength of ibuprofen was 230 nm,the detection wavelength of acetolofenac and diclofenac sodium was 278 nm,and the detection wavelength of the other 16 nonsteroidal substances was 245 nm.The mass concentrations of 19 NSAIDs had a good linear relationship with the corresponding chromatographic peak areas in the range of 5-200μg/mL,the correlation coefficients were all more than 0.9995,and the detection limits were 0.2-8 mg/kg.The average recoveries of spiking in theaqueous solution and gel matrix of the blank sample were 93.1%-110.9%and 91.3%-108.1%,respectively,and the relative standard deviations of the determination results were 0.2%-3.5%and 0.6%-4.2%(n=6).The method is suitable for the determination of 19 NSAIDs in cosmetics.
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