Determination of 42 glucocorticoids in infant eczema products by auto-solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry

doi:10.3724/SP.J.1123.2017.10035

Abstract

Abstract: A method was developed for the determination of 42 glucocorticoids in infant eczema products by auto-solid phase extraction-high performance liquid chromatography-tandem mass spectrometry (ASPE-UHPLC-MS/MS).The analytes were extracted by acetonitrile after dispersing in saturated sodium chloride solution.Macromolecules matrix were precipitated by adding potassium and zinc acetate, and then purified by HLB SPE column.The chromatographic separations were performed on a DIKMA EndeavorsilTM C18 column (100 mm×2.1 mm, 1.7 μm).Acetonitrile and 0.1%(v/v) formic acid aqueous solution were used as the mobile phases.Electrospray ionization (ESI) source was operated in the positive mode using multiple reaction monitoring (MRM) scanning mode.The results were quantified by external standard method.The correlation coefficients of linear calibration curves were greater than 0.998 in the corresponding mass concentration ranges.The average recoveries at three spiked levels ranged from 78.7% to 101.5%, and the relative standard deviations (RSDs) were 2.0%-8.8%(n=6).The LODs (S/N ≥ 3) and LOQs were 0.002-0.031 mg/kg and 0.0007-0.103 mg/kg, respectively.The method is simple, rapid, sensitive, and reliable, and can be used for the detection of glucocorticoids in infant eczema products.

Key words: auto-solid phase extraction (ASPE), glucocorticoid, infant eczema products, ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS-MS)

CLC Number:

O658

PAN Xiaohong, YIN Shuai, LIU Yuling, LONG Lingyun, ZHAO Wei, MENG Qingyu. Determination of 42 glucocorticoids in infant eczema products by auto-solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(4): 356-361.

References

[1] Wu G R, Liang Q S, Xu F B, et al. China Medical Engineering, 2012, 20(5):14 吴谷茸, 梁庆生, 徐冯波, 等. 中国医学工程, 2012, 20(5):14
[2] Wahn U. Allergy, 2000, 55:591
[3] Halken S, Host A. Allergy, 2000, 55:793
[4] Wen Z M. Diagnosis and Treatment of Allergic Diseases (from Infant to Adult). Beijing:Chinese Medical Science and Technology Press, 1998:249 文昭明. 变态反应疾病的诊治(从婴儿到成人). 北京:中国医药科技出版社, 1998:249
[5] Meng M L, Bin B P. Clinical Journal of Chinese Medicine, 2011, 3(1):55 蒙美禄, 宾博平. 中医临床研究, 2011, 3(1):55
[6] Dai J X, Bao Y X, Han L S. Infantile Asthma. Shanghai:Shanghai Science and Technology Education Press, 2006:11 戴家熊, 鲍一笑, 韩连书. 婴儿哮喘. 上海:上海科技教育出版社, 2006:11
[7] Sausenthaler S, Rzehak P, Chen C M, et al. J Investig Allergol Clin Immunol, 2009, 19(6):481
[8] Zhang C. Journal of Community Medicine, 2013, 11(6):54 张翠. 社区医学杂志, 2013, 11(6):54
[9] Yan H Y. Capital Medicine, 2010(8):16 鄢红瑜. 首都医药, 2010(8):16
[10] China Food and Drug Administration. No. 268 Bulletin of China Food and Drug Administration on Safety and Technical Standards for Cosmetics (2015 Edition). (2015-12-23)[2017-11-02]. http://www.sda.gov.cn/WS01/CL0087/140161.html 国家食品药品监督管理总局. 国家食品药品监督管理总局关于发布化妆品安全技术规范(2015年版)的公告(2015年第268号). (2015-12-23)[2017-11-02]. http://www.sda.gov.cn/WS01/CL0087/140161.html
[11] 76/768/EEC
[12] Wang W P, Zhang M Y, Lin J, et al. Chinese Journal of Pharmaceutical Analysis, 2013, 33(5):837 王伟萍, 张明玥, 蔺娟, 等. 药物分析杂志, 2013, 33(5):837
[13] Li Q, Zhang X G, Ma J M, et al. Journal of Instrumental Analysis, 2016, 35(2):179 李强, 张晓光, 马俊美, 等. 分析测试学报, 2016, 35(2):179
[14] Luo H T, Huang X L, Wu H Q, et al. Journal of Instrumental Analysis, 2016, 35(2):119 罗辉泰, 黄晓兰, 吴惠勤, 等. 分析测试学报, 2016, 35(2):119
[15] Luo H T, Huang X L, Wu H Q, et al. Chinese Journal of Chromatography, 2017, 35(8):816 罗辉泰, 黄晓兰, 吴惠勤, 等. 色谱, 2017, 35(8):816
[16] GB/T 24800.2-2009
[17] Qiu B Y, Gao Z H. Modern Cosmetics Science and Technology. Beijing:China Light Industry Press, 2016:2065 邱炳毅, 高志红. 现代化妆品科学与技术. 北京:中国轻工业出版社, 2016:2065
[18] Yu J H. Qinghai Medical Journal, 2012, 42(7):55 余金华. 青海医药杂志, 2012, 42(7):55
[19] Gao Y, Lu N, Zhi L L, et al. Chinese Journal Aesthetic Medicine, 2015, 24(3):77 高莹, 鲁楠, 职蕾蕾, 等. 中国美容医学, 2015, 24(3):77
[20] Zuo X Y. The Medical Journal of the Present Clinical, 2015, 28(6):1821 左晓玥. 当代临床医刊, 2015, 28(6):1821
[21] Xiang P, Shen M, Zhuo X Y. Journal of Instrumental Analysis, 2009, 28(6):753 向平, 沈敏, 卓先义. 分析测试学报, 2009, 28(6):753