LC-MS/MS法测定保湿霜中皮质激素含量

IF 0.4 Q4 SPECTROSCOPY Mass Spectrometry Letters Pub Date : 2016-03-31 DOI:10.5478/MSL.2016.7.1.26
Sumin Park, G. Choi, S. Lee, Hyun Jeong Kim, H. Yum, K. Paeng
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引用次数: 1

摘要

采用液相色谱-串联质谱法(MS/ MS)同时测定润肤露中3种皮质激素(丙酸氯倍他索、二丙酸倍他米松、丙酸氟替卡松)的含量。采用液液萃取(LLE)法制备样品。保湿霜含有乳化剂,它能形成胶束。为了提高胶束中皮质激素的提取效率,在样品制备的LLE提取阶段,在不同pH条件下,采用新开发的可去除保湿剂基质效应的优化提取条件。因此,提取前在保湿液样品中加入10µL的1m HCl可以提高提取效率。为了进行定量分析,我们制作了包含所有目标皮质类固醇特异性转变的SRM表。对该方法进行了线性度、准确度、精密度、检出限、定量限和回收率的验证。在标定标准范围内得到0.99 r2以上的值。得到了较好的精度和精密度。所有检测的皮质类固醇lod均低于31 ng/mL, loq估计低于94 ng/mL。
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Determination of Corticosteroids in Moisturizers by LC-MS/MS
Simultaneous determination of three corticosteroids (clobetasol propionate, betamethasone dipropionate, fluticasone propionate) in moisturizers was performed by using liquid chromatography (LC) coupled with tandem mass spectrometry (MS/ MS). Sample preparation was conducted by the liquid-liquid extraction (LLE). Moisturizers include emulsifying agent and it forms micelles. In order to improve the extraction efficiency of corticosteroids trapped in micelle, newly developed-optimized extraction conditions which can remove the matrix effect from moisturizers was applied with various pH conditions in LLE extraction stage of sample preparation. Thus, the addition of 10 µL of 1 M HCl into moisturizers sample before extraction could improve the extraction efficiency. For the quantitative analysis, SRM table that contained specific transition of all of target corti- costeroids was created. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), limit of quantization (LOQ) and recovery. Over the 0.99 r 2 value was obtained in calibration standard range. Effective accuracy and pre- cision were also obtained. LODs were below 31 ng/mL and LOQs were estimated below 94 ng/mL for all corticosteroids tested.
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来源期刊
CiteScore
0.90
自引率
20.00%
发文量
0
审稿时长
6 weeks
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