超高效液相色谱-串联质谱法同时测定化妆品中21种糖皮质激素

目的:建立快速、准确、灵敏检测化妆品中添加的21种糖皮质激素:曲安西龙、波尼松龙、氢化可的松、波尼松、可的松、倍他米松、地塞米松、氟米松、倍氟米松、波尼松龙醋酸酯、氢化可的松醋酸酯、氟米龙、地夫可特、氟氢可的松醋酸酯、甲基泼尼松龙醋酸酯、布地奈德、泼尼卡酯、安西奈德、哈西奈德、倍氟米松双丙酸酯、地塞米松醋酸酯的分析方法。方法:样品用饱和氯化钠溶液分散,用乙腈从分散液中提取激素类药物,用亚铁氰化钾和醋酸锌从提取液中沉淀大分子基质,经Oasis HLB固相萃取小柱富集净化;采用SHIMADZU Shim-pack XR-ODS色谱柱(3.0 mm×75 mm,1.8 μm),水(含0.1%乙酸)(A)-乙腈(含0.1%乙酸)(B)梯度洗脱,流速0.2 mL·min^-1;离子源为ESI源,正离子扫描模式,多级反应监测测定。结果:该法各组分的平均回收率为85.7%~100.0%,RSD为2.6%~8.9%,方法检出限为0.005~0.053 μg·g^-1。结论:该法能满足检测化妆品中21种糖皮质激素的需要。

Objective:To establish a quick,accurate,sensitive method for analysis of 21 glucocorticoids (triamcinolone,prednisolone,hydrocortisone,prednisone,cortisone,betamethasone,dexamethasone,flumethasone,beclomethasone,prednisolone,21-acetate,fluoromethalone,hydrecortisone 21-acetateby ,deflazacort,fludrocortisone 21-acetate,methylprednisolone 21-cetate,budesonide,dexamethasone-21acetate,prednicarbate,halcinonide,amcinonide,beclometasone dipropionate) in cosmetics by UPLC-MS/MS.Methods:Sample was dispersed with saturated sodium chloride solution,extracted by acetonitrile scattered;then macromolecules from matrix were precipitated with ferrocyanatum kalium and zinc acetate,and finally extracted,enriched and purified by Oasis HLB macromolecular matrix solid-phase extraction and columella.The chromatographic was performed using a SHIMADZU Shim-pack XR-ODS analysis column(3.0 mm×75 mm,1.8 μm) with gradient elution of water(including 0.1% acetic acid)(A)-acetonitrile(including 0.1% acetic acid)(B) at a flow rate of 0.2 mL·min^-1;ESI source was applied and operated in positive ion mode and multiple reaction monitoring(MRM).Results:The recoveries were 85.7%-100.0%,and the RSDs were 2.6%-8.9%;The method detection limits were 0.005-0.053 μg·g^-1.Conclusion:The method can be used to detect 21 glucocorticoids in cosmetics.

1 WANG Chao(王超),MA Qiang(马强),WANG Xing(王星),et al.Simultaneous determination of 16 hormones in cosmetics by liquid chromatography tandem mass spectrometry(液相色谱-串联质谱法同时测定化妆品中的16种激素).Chin J Anal Chem(分析化学),2007,35(9):1257
2 ZHANG Ya-jun(张雅军),LI Xiao-dong(李晓东).Studies on identification of seven glucocorticoids by HPLC-MS/MS(液相色谱-串联质谱鉴别7种糖皮质激素的方法研究).J Instrum Anal(分析测试学报),2007,26[Suppl(增刊)]:67
3 WU Zhong-pin(武中平),LU Jian(卢剑),GAO Wei(高巍),et al.Determination of various hormones in cosmetics by liquid chromatography together with mass spectrometry(液相色谱-串联质谱法测定化妆品中多种激素).Chin Surf Det Cosm(日用化学工业),2010,40(2):153
4 TIAN Yuan(田媛),FENG Shu-dan(冯舒丹),HUANG Mei-hua(黄美花),et al.LC-MS/MS determination of glucocorticoids illegally added into cosmetics(化妆品中糖皮质激素类非法添加物的LC-MS/MS分析).J Chin Pharm Univ(中国药科大学学报),2011,42(1):53
5 WU Da-nan(吴大南),ZHENG He-hui(郑和辉),WANG Ping(王萍),et al.Determination of 8 glucocorticoids in cosmetics by ultra performance liquid chromatography(超高效液相色谱法检测化妆品中8种糖皮质激素).Chin J Health Lab Technol(中国卫生检验杂志),2008,8(2):197
6 LIU Jun(刘军).Determination of glucocorticoids in cosmetics by spectrophotometry(分光光度法测定化妆品中甾体激素含量).Chin J Health Lab Technol(中国卫生检验杂志),2000,10(5):571
7 ZHAO Xiao-ya(赵晓亚),LIN Yan-fei(林雁飞),HU Xiao-zhong(胡小钟),et al.Determination of 9 glucocorticoids in cosmetics by reversed phase high performance liquid chromatography(反相高效液相色谱法同时测定化妆品中的9种糖皮质激素).Chin J Anal Lab(分析试验室),2009,28(2):111
8 TIAN Yuan(田媛),FENG Shu-dan(冯舒丹),HUANG Mei-hua(黄美花),et al.LC-MS/MS determination of glucocorticoids illegally added into cosmetics(化妆品中糖皮质激素类非法添加物的LC-MS/MS分析).J China Pharm Univ(中国药科大学学报),2011,42(1):53
9 WANG Chuan-xian(王传现),LIU Gang-yi(刘罡一),NI Xin-lu(倪昕路),et al.Determination of glucocorticoids in cosmetics by HPLC-MS/MS(高效液相色谱-串联质谱法检测化妆品中糖皮质激素类违禁药物).Anal Instrum(分析仪器),2008(6):23
10 WU Wei-qun(吴维群),SHEN Chao-ye(沈朝烨),YANG Yu-lin(杨玉林),et al.Determination of sex hormones in liquid cosmetics by gas chromatography-mass spectrometry(GC-MS联用技术检测水性化妆品中性激素成分的方法研究).Chin J Environ Occup Med(环境与职业医学),2004,21(4):307.
11 GB/T 24800.2.National standards of The People's Republic of China(中华人民共和国国家标准).Determination of 41 glucocorticoids in cosmetics by LC-MS-MS and TLC method(化妆品中四十一种糖皮质激素的测定液相色谱/串联质谱法和薄层层析法).2009