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通过式高效净化/超高效液相色谱-串联质谱法测定化妆品中73种糖皮质激素
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刘红,杨飘飘,李丽霞 1.湖北省药品监督检验研究院2.湖北省药品质量检测与控制工程技术研究中心 
中文摘要:建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定化妆品中73种糖皮质激素的分析方法。样品采用饱和氯化钠分散,乙腈超声提取,经PRiME HLB固相萃取柱(60 mg/3 mL)净化,采用Waters Cortecs C18色谱柱(150 mm×2.1 mm,2.7 μm)分离,以0.1%乙酸溶液-乙腈为流动相梯度洗脱。在电喷雾离子源正离子模式下,采用多反应监测(MRM)扫描方式测定,外标法定量。结果表明,73种糖皮质激素在各自的质量浓度范围内均呈良好线性关系,相关系数(r)均大于 0.99,定量下限(LOQ)为0.1~0.3 μg/g。在1LOQ、2LOQ、5LOQ 3个加标水平下,73种糖皮质激素的回收率为 73.3%~119%,相对标准偏差(RSD)为0.40%~18%。该方法快速、准确、高效,可作为化妆品中73种糖皮质激素的筛查方法。
中文关键词:化妆品  糖皮质激素  超高效液相色谱-串联质谱(UPLC-MS/MS)
 
Detection of 73 Glucocorticoids in Cosmetics by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Pass-through Column Purification
Abstract:An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the determination of 73 glucocorticoids in cosmetics.Samples were dispersed with saturated sodium chloride and ultrasonically extracted with acetonitrile,then purified with a PRiME HLB SPE column(60 mg/3 mL) and separated on a Waters Cortecs C18 column(150 mm×2.1 mm,2.7 μm) by gradient elution using 0.1% acetic acid solution and acetonitrile as mobile phases.The analysis was performed with electrospray ion source in positive ion mode under multi-reaction monitoring(MRM) mode,and the results were quantified by external standard method.Results showed that there were good linear relationships for 73 glucocorticoids in cosmetics in their respective concentration ranges with correlation coefficients(r) higher than 0.99.The limits of quantitation(LOQ) were in the range of 0.1-0.3 μg/g.The average recoveries for 73 glucocorticoids at three spiked levels of 1LOQ,2LOQ and 5LOQ ranged from 73.3% to 119%,with relative standard deviations(RSD) of 0.40%-18%.The method was rapid and accurate,and could be used as a screening approach for 73 glucocorticoids in cosmetics.
Key Words:cosmetics  glucocorticoids  ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
引用本文:刘红,杨飘飘,李丽霞.通过式高效净化/超高效液相色谱-串联质谱法测定化妆品中73种糖皮质激素[J].分析测试学报,2020,39(9):1112-1119.
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