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高效液相色谱法测定化妆品中11a-孕酮和11a-孕酮醋酸盐

Determination of 11a-progesterone and 11a-progesterone acetate in cosmetics by high performance liquid chromatography method

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目的 建立凝胶渗透色谱净化液相色谱法检测 11a-孕酮、11a-孕酮醋酸盐二种激素的分析方法,为市场监管和企业质量控制提供技术支撑.方法 样品经乙酸乙酯提取,使用乙酸乙酯:正己烷=1:1 作为淋洗液,经凝胶渗透色谱(gel permeation chromatography,GPC)净化,收集 12~20 min淋洗液,淋洗液经旋转蒸发旋得到待测净化液.采用乙腈:水=45:55 作为流动相、C18(250×4.6 mm)色谱柱进行分离、二级管阵列检测器对最大吸收波长为 245 nm的 11a-孕酮、11a-孕酮醋酸盐两种激素进行同时测定.结果 该方法线性相关系数在0.995 以上,三种代表性化妆品加标回收率分别为 90.0%~102.6%、85.1~102.7%,相对标准偏差(relative standard deviation,RSD)分别为 0.7%~2.5%、0.1%~8.7%,方法检出限分别为 0.3 mg/kg、0.6 mg/kg,定量限分别为 1.0 mg/kg、2.0 mg/kg.结论 该方法操作简单、定性可靠、定量准确,可用于化妆品中禁用激素 11a-孕酮、11a-孕酮醋酸盐含量测定.
Objective To study the detection method of 11a-progesterone and 11a-progesterone acetate by gel permeation chromatography and liquid chromatography,and to provide technical support for market supervision and enterprise quality control.Methods Samples are extracted by ethyl acetate;use 1:1 ethyl acetate:hexane as eluent;purify by gel permeation chromatography(GPC)method;collect the eluent for 12~20 min;obtain the purified solution from eluent by rotary evaporation;wait for the determination of liquid chromatography.Use 45:55 acetonitrile:water as mobile phase;use C18(250×4.6 mm)chromatographic column for separation;use photo diode array detector for the determination of 11a-progesterone and 11a-progesterone acetate at 245 nm.Results The linear correlation coefficient of this method is above 0.995,the recovery rate is 90.0%~102.6%and 85.1~102.7%,the relative standard deviation(RSD)is 0.7%~2.5%and 0.1%~8.7%,the limit of detection is 0.3 mg/kg and 0.6 mg/kg,and the limit of quantification is 1.0 mg/kg and 2.0 mg/kg.Conclusion The method is simple,reliable and accurate,and can be used for the determination of 11a-progesterone acetate and 11a-progesterone acetate in cosmetics.

high performance liquid chromatography11a-progesterone11a-progesterone acetatecosmetics

王丁林、顾宇翔

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上海市质量监督检验技术研究院,上海 200233

高效液相色谱法 11a-孕酮 11a-孕酮醋酸盐 化妆品

2024

实验室检验
中国检验检测学会

实验室检验

ISSN:2097-261X
年,卷(期):2024.2(2)
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