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作 者:肖庚鹏[1] 罗春丽 黄优生[1] 罗香[1] XIAO Gengpeng;LUO Chunli;HUANG Yousheng;LUO Xiang(Analysis and Testing Research Institute of Jiangxi Province,Nanchang 330029)
出 处:《分析试验室》2021年第5期568-572,共5页Chinese Journal of Analysis Laboratory
基 金:江西省科技计划项目(20151BBG70050)资助。
摘 要:建立了以2,4-二硝基氟苯(DNFB)为衍生试剂,柱前衍生-高效液相色谱测定化妆品中牛磺酸的方法。水溶性化妆品和水包油型化妆品用水分散、超声提取、离心过滤后直接衍生进样;油包水型化妆品先用乙腈预分散后再用水稀释、超声提取、离心过滤后经衍生进样。分别从衍生试剂的选择、常见干扰因素的排除、衍生试剂添加量、及预分散溶剂的选择和添加量等方面进行了方法优化。采用Ultimate Amino Acid色谱柱(4.6 mm×250 mm,5μm)分离,柱温32℃,以50 mmol/L乙酸钠溶液-乙腈(1:1,V/V)为流动相A和50 mmol/L乙酸钠溶液为流动相B进行梯度洗脱,流速1.0 mL/min,检测波长355 nm,进样量20μL。结果表明,目标物质量浓度在5~100 mg/L范围内线性良好;检出限(LOD)为6 mg/kg;定量限(LOQ)为20 mg/kg;在3个添加水平下目标物的加标平均回收率为95.6%~103.7%;相对标准偏差(RSD)为1.1%~4.4%。该方法能够满足化妆品中牛磺酸的测定。Based on different formula structures,a method was established for the determination of taurine in cosmetics with 2,4-dinitrofluorobenzene as pre-column derivate reagent by high performance liquid chromatography(HPLC).Water-soluble cosmetics and oil-in-water cosmetics were diluted with water,ultrasonic extraction,centrifugal filtration and then directly derived and determined by HPLC;water-in-oil cosmetics were pre-dispersed with acetonitrile,diluted with water,ultrasonic extraction,centrifugal filtration,then derivatized and determined by HPLC.The methods were optimized in terms of the selection and addition amount of derivatization reagents,the possible interferences of the matrix,and the selection and addition amount of pre-dispersing solvents.The derivatives were separated using an Ultimate Amino Acid(4.6 mm×250 mm,5μm)chromatographic column,and the mobile phases for gradient elution with 50 mmol/L sodium acetate-acetonitrile(1∶1,V/V)and 50 mmol/L sodium acetate aqueous solution.The column temperature was 32℃,the flow rate was 1.0 m L/min,the detection wavelength was 355 nm,and the injection volume was 20μL.Quantification was performed using external standards.Good linearity was obtained in the concentration range of 5.0-100 mg/L with correlation coefficient of0.994,the limit of detection(LOD)was 6 mg/kg,and the limit of quantification(LOQ)was 20 mg/kg.The average recoveries of the target at the three levels were in the range of 95.6%-103.7%with the relative standard deviations(RSDs)within 1.1%-4.4%.The results showed that the analysis method meet the requirements for efficient analysis of taurine in cosmetics.
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