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作 者:张伟清[1] 侯俐南 李彬 刘慧锦 王海燕[1] ZHANG Wei-qing;HOU Li-nan;LI Bin;LIU Hui-jin;WANG Hai-yan(National Institutes for Food and Drug Control,Beijing 100050,China)
出 处:《日用化学工业》2021年第6期577-582,共6页China Surfactant Detergent & Cosmetics
摘 要:建立了超高效液相色谱-三重四级杆质谱法(UPLC/MS-MS)测定人参化妆品中人参功效成分(人参皂苷Rg1,人参皂苷Re),并用该方法对市售28批样品进行风险监测。样品采用甲醇超声提取法,以0.05%甲酸水溶液-0.05%甲酸乙腈溶液为流动相,梯度洗脱,ACQUITY UPLC BEH C_(18) (2.1 mm×100 mm×1.7μm)色谱柱分离,以UPLC/MS-MS负离子模式检测。同时对样品前处理条件及色谱-质谱条件进行优化,并完成方法学验证。结果表明,两种目标化合物在0.1~50 ng/mL及0.5~200 ng/mL质量浓度范围内呈良好线性关系,R~2大于0.999 6;LOD为0.001 7~0.003 0μg/g (S/N=3);在膏霜、乳液、洗护类基质中加标回收率为81.87%~94.45%,相对标准偏差小于5.64%(n=6)。该方法适用于人参化妆品中人参功效成分的测定。A method was established for the determination of ginseng functional components(ginsenoside Rg1,ginsenoside Re)in ginseng cosmetics with ultra-high performance liquid chromatography triple quadrupole mass spectrometry(UPLC/MS-MS).This method was used to monitor the risk of 28 batches of samples sold on the market.The samples were extracted by methanol ultrasonic method.The mobile phase was 0.05%formic acid aqueous solution-0.05%formic acid acetonitrile solution,and the gradient elution was carried out.The samples were separated on the ACQUITY UPLC BEH C18(2.1 mm×100 mm×1.7μm)column and detected by UPLC/MS-MS negative ion mode.At the same time,the pretreatment conditions and UPLC/MS-MS conditions were optimized and the method was verified.The results show that the method shows good linearity in the concentration range of 0.1-50 ng/mL and 0.5-200 ng/mL,with R2 no less than 0.9996.The limits of detection are in the range of 0.0017-0.0030μg/g(S/N=3).The average recoveries in sample matrix of cream,lotion and shampoo are from 81.87%to 94.45%,with relative standard deviations(RSDs)less than 5.64(n=6).This method is suitable for the determination of ginseng functional components in ginseng cosmetics.
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