Rapid determination of 66 antibiotics in cosmetics using ultra high performance liquid chromatography-linear ion trap/Orbitrap mass spectrometry

doi:10.3724/SP.J.1123.2018.01041

Abstract

Abstract:

A rapid screening and determination method, in conjunction with a database for confirmation, was established based on 66 antibiotic compounds using ultra-high performance liquid chromatography-linear ion trap/Orbitrap high resolution mass spectrometry (UPLC-LTQ/Orbitrap MS). The analytes were extracted with acetonitrile using ultrasonic extraction. The separation was performed on a C18 column (100 mm×2.1 mm, 1.8 μm) with a gradient elution of 0.1% (v/v) formic acid and acetonitrile. The retention time and accurate mass of the precursor ion were used for rapid screening in positive ionization mode, with the fragment ions obtained by higher energy collisional dissociation used for confirmation. The results indicated that each compound showed good linearity with a correlation coefficient of R²>0.99. The limits of detection (LODs) were in the range 2-4 μg/kg, and the limits of quantification (LOQs) were in the range 5-10 μg/kg. The average recoveries at three levels (1LOQ, 10LOQ, and 30LOQ) were between 58.2% and 119.1%, and the relative standard deviations (RSDs) were between 1.03% and 11.9%. The method is simple, rapid, reliable, and accurate, which is suitable for rapid screening and determination of the 66 antibiotic compounds in cosmetics.

Key words: antibiotics, cosmetics, linear ion trap/Orbitrap high resolution mass spectrometry(LTQ/Orbitrap MS), ultra-high performance liquid chromatography(UPLC)

CLC Number:

O658

LI Hongying, SHEN Huadan, FANG Jiangji, ZHANG Jingya, DING Xiaoping. Rapid determination of 66 antibiotics in cosmetics using ultra high performance liquid chromatography-linear ion trap/Orbitrap mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(7): 643-650.

References

[1] China Food and Drug Administration. Safety and Technical Standards for Cosmetics (2015 Edition). Beijing, 2015 国家食品药品监督管理总局. 化妆品安全技术规范(2015年版). 北京, 2015
[2] Li M H, Kong W J, Yang M H, et al. China Journal of Traditional Chinese Medicine and Pharmacy, 2016, 31(6):2239 李梦华, 孔维军, 杨美华, 等. 中华中医药杂志, 2016, 31(6):2239
[3] Zhu L, Liu Y, Zeng S P, et al. Journal of Instrumental Analysis, 2016, 35(2):185 朱俐, 刘洋, 曾三平, 等. 分析测试学报, 2016, 35(2):185
[4] Chen J, Zheng R, Ji S, et al. Chinese Journal of Analytical Chemistry, 2013, 41(6):931 陈静, 郑荣, 季申, 等. 分析化学, 2013, 41(6):931
[5] Qian Y F, Jia C P. Guangzhou Chemical Industry, 2016, 44(10):150 钱叶飞, 贾昌平. 广州化工, 2016, 44(10):150
[6] Zhang L T, Huang S Y, Yang X, et al. Chinese Journal of Analysis Laboratory, 2015, 34(12):1403 张林田, 黄少玉, 杨晞, 等. 分析试验室, 2015, 34(12):1403
[7] Lu J, Pang Y J, Li Y B, et al. Chinese Journal of Chromatography, 2012, 30(6):641 陆军, 庞燕军, 李彦博, 等. 色谱, 2012, 30(6):641
[8] Jian L H, Zheng R, Zhong J Q, et al. Chinese Journal of Analysis Laboratory, 2014, 33(12):1459 简龙海, 郑荣, 钟吉强, 等. 分析试验室, 2014, 33(12):1459
[9] Meng Q, Zheng R, Wang K. Chinese Journal of Health Laboratory Technology, 2016, 26(6):784 孟茜, 郑荣, 王柯. 中国卫生检验杂志, 2016, 26(6):784
[10] Zhang Y H, Li L L, Wang H M. Chinese Journal of Health Laboratory Technology, 2017, 27(18):2600 张燕惠, 李玲玲, 王红梅. 中国卫生检验杂志, 2017, 27(18):2600
[11] Wu C S, Zhang J L, Qiao Y L, et al. Chinese Chemical Letters, 2011, 22(3):334
[12] Liu Y, Zhang F, Chang Y, et al. Chinese Journal of Pharmaceutical Analysis, 2017, 37(9):1693 刘颖, 张帆, 常艳, 等. 药物分析杂志, 2017, 37(9):1693
[13] Lin L, Zhang Y, Tu X K, et al. Chinese Journal of Chromatography, 2015, 33(3):275 林黎, 张毅, 涂小珂, 等. 色谱, 2015, 33(3):275
[14] Luo H T, Huang X L, Wu H Q, et al. Chinese Journal of Analytical Chemistry, 2017, 45(9):1381 罗辉泰, 黄晓兰, 吴惠勤, 等. 分析化学, 2017, 45(9):1381
[15] Niu Z Y, Luo X, Wang F M, et al. Journal of Chinese Mass Spectrometry Society, 2016, 37(3):201 牛增元, 罗忻, 王凤美, 等. 质谱学报, 2016, 37(3):201
[16] Li X W, Shen B H, Jiang Z, et al. Journal of Forensic Medicine, 2012, 28(1):44 李晓雯, 沈保华, 江峥, 等. 法医学杂志, 2012, 28(1):44
[17] Li Z Y, Wang F M, Niu Z Y, et al. Chinese Journal of Chromatography, 2014, 32(5):477 李兆永, 王凤美, 牛增元, 等. 色谱, 2014, 32(5):477
[18] Wang F M, Niu Z Y, Luo X, et al. Journal of Food Safety and Quality, 2014, 5(12):3911 王凤美, 牛增元, 罗忻, 等. 食品安全质量检测学报, 2014, 5(12):3911
[19] Skrabáková Z, O'Halloran J, van Pelt F N A M, et al. Rapid Commun Mass Spectrom, 2010, 24 (20):2966
[20] 2002/657/EC. Official Journal of the European Communities, 2002, L221:8