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作 者:刁飞燕 李俊婕 吴晓云 刘慧香 于海英 李启艳 DIAO Feiyan;LI Junjie;WU Xiaoyun;LIU Huixiang;YU Haiying;LI Qiyan(Shandong Institute for Food and Drug Control,NMPA Key Laboratory for Quality Control of Cosmetics Raw Material,Jinan Engineering Research Center for Cosmetics of Specialty Plant Resources,Industrial Technology Foundation Public Service Platform,Jinan 250101,China)
机构地区:[1]山东省食品药品检验研究院,国家药品监督管理局化妆品原料质量控制重点实验室,特色植物资源化妆品济南市工程研究中心,产业技术基础公共服务平台,济南250101
出 处:《化学分析计量》2024年第1期41-45,52,共6页Chemical Analysis And Meterage
基 金:山东省企业技术创新项目(202150101110)。
摘 要:建立高效液相色谱法测定化妆品原料中N-乙酰神经氨酸含量的方法。以体积分数为50%的乙酸溶液为水解溶剂,样品于80℃水浴中加热30 min,以CAPCELL PAK SCX柱(250 mm×4.6 mm,5μm)为分析柱,流动相为乙腈-0.1%磷酸水溶液(体积比为80∶20),等度洗脱,流量为1.0 mL/min,柱温为35℃,采用高效液相色谱二极管阵列检测器测定,以色谱峰面积外标法定量。检测波长为205 nm,进样体积为10μL。N-乙酰神经氨酸的色谱峰面积与质量浓度在10.0~500.0μg/ml范围内线性关系良好,相关系数为0.9999,方法检出限为0.12μg/mL,定量限为0.4μg/mL。样品加标平均回收率为97.7%~98.9%,测定结果的相对标准偏差为0.37%~1.36%(n=6)。该方法样品处理简便、高效,适用于化妆品原料中N-乙酰神经氨酸的含量测定。A method for the determination of N-acetylneuraminic acid in raw materials of cosmetics by high performance liquid chromatography was established.Acetic acid solution with a volume fraction of 50%was used as the hydrolysis reagent,the samples were heated in water bath at 80℃for 30 minutes.CAPCELL PAK SCX column(250 mm×4.6 mm,5μm)was used as the analysis column,the mobile phase was acetonitrile-0.1%phosphoric acid aqueous solution(volume ratio was 80:20)for isocratic elution,the flow rate was 1.0 mL/min.The temperature of the column was 35℃.The sample solution was determined by high performance liquid chromatography diode array detector.Quantitative analysis was performed using chromatographic peak area external standard method.The detection wavelength was 205 nm and the injection volume was 10μL.The chromatographic peak area of N-acetylneuraminic acid had a good linear relationship with the mass concentration in the range 10.0-500.0μg/mL,the correlation coefficient was 0.9999,the detection limit of the method was 0.12μg/mL,and the quantification limit was 0.4μg/mL.The average recoveries of sample spiking were 97.7%-98.9%,and the relative standard deviations of the determination results were 0.37%-1.36%(n=6).The method is simple and efficient,which is suitable for the determination of N-acetylneuraminic acid in raw materials of cosmetics.
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