Simultaneous determination of 14 sexual hormones in health care products by ultra performance liquid chromatography-atmospheric pressure chemical ionization-triple quadrupole mass spectrometry

doi:10.3724/SP.J.1123.2018.12039

Abstract

Abstract:

A comprehensive analytical method was developed for the simultaneous determination of 14 sexual hormones in health care products by ultra performance liquid chromatography-atmospheric pressure chemical ionization-triple quadrupole mass spectrometry (UPLC-APCI-MS/MS). The samples were extracted twice with acetonitrile and the extracts were purified using hydrophilic-lipophilic balance (HLB) cartridges. Chromatographic separation was achieved on a Hypersil Gold C18 column (100 mm×2.1 mm, 1.9 μm) by gradient elution with acetonitrile and 10 mmol/L ammonium acetate aqueous solution as the mobile phases. Compounds were detected by APCI-MS/MS with external standard calibration curve method. All the 14 sexual hormones showed a good linear trend in their respective concentration ranges and the correlation coefficients (r) were no less than 0.996. The limits of detection (LODs) ranged from 0.0990 μg/kg to 2.09 μg/kg. The limits of quantification (LOQs) were in the range of 0.495-5.23 μg/kg. The average recoveries of the 14 sexual hormones in the health care product samples ranged from 65.8% to 118.8% at the three spiked levels. The precisions (n=6) ranged from 0.6% to 8.7% (n=6). The method is simple, sensitive, accurate and precise, and is suitable for the determination of the illegal added sexual hormones in the health care products.

Key words: atmospheric pressure chemical ionization (APCI), health care products, sexual hormones, ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS)

CLC Number:

O658

RAO Yakun, LI Zhuo, ZHANG Diyue, DONG Manman, WEI Xinghua, CHEN Dong, ZHANG Yafeng. Simultaneous determination of 14 sexual hormones in health care products by ultra performance liquid chromatography-atmospheric pressure chemical ionization-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, 2019, 37(6): 626-633.

References

[1] Li H L, Si J W, Shen G F. Chinese Journal of Tissue Engineering Research, 2015, 19(7):1077 李洪亮, 司家文, 沈国芳. 中国组织工程研究, 2015, 19(7):1077
[2] Xie G H, Pan X L, Li H, et al. Journal of Nanchang University (Medical Sciences), 2014, 54(10):88 谢贵花, 潘小玲, 李慧, 等. 南昌大学学报(医学版), 2014, 54(10):88
[3] Tan J. The World Clinical Medicine, 2017, 11(12):137 谈军. 世界临床医学, 2017, 11(12):137
[4] Lu L, Wang X H. Chinese Journal of Cell Biology, 2017, 39(4):529 鲁林, 王晓慧. 中国细胞生物学学报, 2017, 39(4):529
[5] Zheng J, Xi C X, Cao S R, et al. Chinese Journal of Chromatography, 2017, 35(12):1257 郑佳, 郗存显, 曹淑瑞, 等. 色谱, 2017, 35(12):1257
[6] Wang Q M, Zhou J H, Zhou J L. Chines General Practice, 2014, 17(30):3638 王泉梅, 周坚红, 周金玲. 中国全科医学, 2014, 17(30):3638
[7] International Agency for Research on Cancer (IARC). A Review of Human Carcinogens. Lyon:World Health Organization Press, 2012
[8] Wang Z L, Zhang J L, Zhang Y N. Modern Scientific Instruments, 2010(4):90 王占良, 张建丽, 张亦农. 现代科学仪器, 2010(4):90
[9] Lu C M, Wang M T, Mou J, et al. Chinese Journal of Chromatography, 2011, 29(6):558 芦春梅, 王明泰, 牟俊, 等. 色谱, 2011, 29(6):558
[10] Lu C M, Wang F H, Hu T T, et al. Chemical Reagents, 2015, 37(3):243 芦春梅, 王风红, 胡婷婷, 等. 化学试剂, 2015, 37(3):243
[11] Chen C J, Zhou Y, Chen X, et al. The Food Industry, 2017, 38(12):292 陈才军, 周勇, 陈翔, 等. 食品工业, 2017, 38(12):292
[12] He X Q.[MS Dissertation]. Chongqing:Chongqing Medical University, 2015 何小琴.[硕士学位论文]. 重庆:重庆医科大学, 2015
[13] Gao F Y, Zhang W B, Guan Y F, et al. Science China Chemistry, 2014, 44(7):1181 高方园, 张维冰, 关亚风, 等. 中国科学:化学, 2014, 44(7):1181
[14] Chai Y F.[PhD Dissertation]. Hangzhou:Zhejiang University, 2013 柴云峰.[博士学位论文]. 杭州:浙江大学, 2013
[15] Shi L K, Yang J, Zhang X T, et al. Chemical Analysis and Meterage, 2014, 23(4):99 石龙凯, 杨进, 张小涛, 等. 化学分析计量, 2014, 23(4):99
[16] Xie J S, Ge Q H. Chinese Journal of Pharmaceutical Analysis, 2008, 28(8):1386 谢家树, 葛庆华. 药物分析杂志, 2008, 28(8):1386
[17] Gao W, Stalder T, Kirschbaum C. Talanta, 2015, 143:353
[18] Mezzullo M, Fazzini A, Gambineri A, et al. J Clin Chem Lab Med, 2017, 55(9):1315
[19] Xu Y J, Tian X H, Zhang X Z, et al. Journal of Instrumental Analysis, 2010, 29(2):152 徐英江, 田秀慧, 张秀珍, 等. 分析测试学报, 2010, 29(2):152
[20] Xiong S. Physical Testing and Chemical Analysis Part B:Chemical Analysis, 2018, 54(2):142 熊爽. 理化检验(化学分册), 2018, 54(2):142
[21] Waters Beijing Laboratory. Environmental Chemistry, 1998, 17(6):606 Waters公司北京实验室. 环境化学, 1998, 17(6):606
[22] Zhou Y B, Li L, Wu Y T, et al. Modern Preventive Medicine, 2018, 45(22):4144 周贻兵, 李磊, 吴玉田, 等. 现代预防医学, 2018, 45(22):4144
[23] Tao D L, Bai H, Li Q. Modern Food, 2018(21):103 陶大利, 白鹤, 李琴. 现代食品, 2018(21):103
[24] Wang Y. Food Science and Technology, 2017, 42(6):270 王颖. 食品科技, 2017, 42(6):270
[25] Zhu Z J, Liu H, Ning Q Q, et al. Chinese Journal of Chromatography, 2019, 37(1):8 朱之烔, 柳菡, 宁倩倩, 等. 色谱, 2019, 37(1):8
[26] Wang C C.[MS Dissertation]. Jinan:Shandong University, 2017 王晨晨.[硕士学位论文]. 济南:山东大学, 2017
[27] Ran Y Z, Qi W X, Li J, et al. Environmental Chemistry, 2018, 37(2):255 冉韵竹, 齐维晓, 李静, 等. 环境化学, 2018, 37(2):255
[28] Chen M, Guo X Y, Wang Z J, et al. Physical Testing and Chemical Analysis Part B:Chemical Analysis, 2018, 54(6):669 陈萌, 郭项雨, 王志娟, 等. 理化检验(化学分册), 2018, 54(6):669