超高效液相色谱-串联质谱法测定化妆品中同分异构体构型糖皮质激素
目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定化妆品中同分异构体构型糖皮质激素(glucocorticoids, GCs)的分析方法。方法 样品经饱和氯化钠分散、乙腈提取, 亚铁氰化钾-醋酸锌沉淀大分子基质后, 通过分散固相萃取技术(QuEChERS)净化。以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱, 采用多反应监测模式(multiple reaction monitoring, MRM)对美白祛斑类化妆品中同分异构体构型糖皮质激素进行定量和定性检测。结果 本方法完成了对糖皮质激素中最难以分离的差向同分异构体倍他米松、地塞米松以及它们的衍生物倍他米松醋酸酯、地塞米松醋酸酯的分离检测。在5.0、10和20 μg/kg添加水平时的回收率为78.6%~102.7%, 相对标准偏差小于10.60%(n=6), 方法定量限为6.0 μg/kg。结论 该方法快速、稳定、灵敏度高、选择性好, 适合分析检测化妆品中非法添加的GCs类化合物。
Objective To establish a method for the determination of isomer configuration glucocorticoids in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry. Methods The sample was dispersed by saturated sodium chloride, extracted by acetonitrile and precipitated macromolecular matrix by potassium ferrocyanide and zinc acetate. Matrix solid-phase dispersion extraction (QuEChERS) was used for purification. Gradient elution was performed with 0.1% formic acid (A) and acetonitrile (B) as mobile phase, and multiple reaction monitoring (MRM) was for the quantitative and qualitative of the isomer configuration glucocorticoids in whitening cosmetics and qualitative testing. Results The method accomplished the separation and detection of the isomeric isomers of betaperdone, dexamethasone and their derivatives, betamethasone acetate and dexamethasone acetate, which were the most difficult to separate in glucocorticoids. The recoveries at the addition levels of 5.0, 10 and 20 μg/kg were 78.6%-102.7%, and the relative standard deviations were less than 10.60% (n=6). The limit of quantification was 6.0 μg/kg. Conclusion This method is fast, accurate, sensitive and reliable, which is suitable for the analysis and detection of illegally added GCs compounds in cosmetics.
标题：超高效液相色谱-串联质谱法测定化妆品中同分异构体构型糖皮质激素
英文标题：Determination of isomer configuration glucocorticoids in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry
作者：
赵洋 吉林省食品检验所;吉林省安信食品技术服务有限公司
王婷 吉林省食品检验所;吉林省安信食品技术服务有限公司
华蕾 吉林省食品检验所
王庆峰 吉林省食品检验所
包懿 吉林省食品检验所
刘斌 吉林省食品检验所
周欣蕊 吉林省食品检验所;吉林省安信食品技术服务有限公司
中文关键词:糖皮质激素,超高效液相色谱-串联质谱法,多重保留分离机制,分散固相萃取技术,
英文关键词:glucocorticoids,high performance liquid chromatography-tandem mass spectrometry,multiple chromatography retention mechanisms,matrix solid-phase dispersion extraction,
发表日期：2019-02-01
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