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作 者:于海英 牛水蛟 张良雨 林钰镓 杨茜 李启艳 YU Haiying;NIU Shuijiao;ZHANG Liangyu;LIN Yujia;YANG Qian;LI Qiyan(Shandong Institute for Food and Drug Control/NMPA Key Laboratory for Quality Control of Cosmetics Raw Material,Jinan 250101,China;Sanyo Fine Trading Co.,Ltd.,Beijing 100176,China)
机构地区:[1]山东省食品药品检验研究院/国家药监局化妆品原料质量控制重点实验室,济南250101 [2]三耀精细化工品销售(北京)有限公司,北京100176
出 处:《理化检验(化学分册)》2025年第1期28-31,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:国家药品监督管理局化妆品标准研究(2021-BZ-014);山东省药品监督管理局药品医疗器械化妆品检验检测能力提升项目(SDNMPAFZLY202205);山东省企业技术创新项目(202150101110)。
摘 要:提出了高效液相色谱-水凝粒子激光计数检测器法测定抗皱类化妆品中玻色因含量的方法。取0.25 g抗皱类化妆品置于50 mL离心管中,加入3 mL甲醇,涡旋1 min,加水至25 mL,超声15 min,摇匀,过0.45μm滤膜,滤液上机分析。以CAPCELL PAK ADME-HR S5色谱柱为固定相,以不同体积比的0.1%(体积分数)甲酸溶液-乙腈混合液为流动相进行梯度洗脱,水凝粒子激光计数检测器测定。结果表明,玻色因的质量浓度在10~1 000 mg·L^(-1)内与对应的非对映异构体的峰面积之和呈线性关系,检出限(3S/N)为0.013%(质量分数)。样品精密度试验所得测定值的相对标准偏差(n=6)小于2.0%,按照标准加入法进行回收试验,回收率为99.5%~100%。方法用于测定实际抗皱类化妆品中玻色因的含量,检出量为2.33%~9.89%(质量分数)。A method for determination of pro-xylane in anti-wrinkle cosmetics by high performance liquid chromatography with water condensation particle laser counting detector was proposed.0.25 g of anti-wrinkle cosmetics was taken and placed in a 50 mL-centrifuge tube.3 mL of methanol was added,and the mixture was vortexed for 1 min.The solution was made its volume up to 25 mL with water,and ultrasound for 15 min.The mixed solution was shaken well and passed through a 0.45μm filter membrane.The filtrate was analyzed by the instrument.CAPCELL PAK ADME-HR S5 chromatographic column was used as the stationary phase and the mixed solution composed of 0.1%(volume fraction)formic acid solution and acetonitrile at different volume ratios was used as the mobile phase for gradient elution.The solution was determined by water condensation particle laser counting detector.As shown by the results,linear relationship between the corresponding the sum of peak areas of diastereomers and mass concentration of pro-xylane was kept in the range of 10-1000 mg·L^(-1),with detection limits(3S/N)of 0.013%(mass fraction).RSDs(n=6)of the determined values of test of sample for precision was less than 2.0%.Test for recovery was made according to the standard addition method,giving results in the range of 99.5%-100%.This method was used to determine the pro-xylane in actual anti-wrinkle cosmetics,with detection amounts in the range of 2.33%-9.89%(mass fraction).
关 键 词:高效液相色谱法 水凝粒子激光计数检测器 抗皱类化妆品 玻色因
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