Abstract:The objective is to use orthogonal experiment to optimize the pretreatment on the determination of serum cholesterol and its markers by GC-MS. And then the method is evaluated in a methodological perspective. The methodis to Use L16(211) orthogonal experiment design to observe the influence of three key steps,althogether seven factors of pretreatment, which are saponification (KOH ethanol solution concentration, temperature and time), extraction (dose) and derivatization (temperature , time and dose). As for the results,the conditions of optimal pretreatment are as follows:the ethanol solution is 1 mol·L-1 KOH, the saponification temperature is 70 ℃;the saponification time is 60 min;the Solvent quantity is 2 mL;the derivatization temperature is 70 ℃;the derivatization time is 60 min,and the derivatization agent is 100 μL. Through the optimization by orthogonal design and methodological evaluation, the determination of serum cholesterol and its markers by GC-MS is excellent in terms of accuracy and precision, and methodological evaluation indexes are better than those reported in other papers.
张 钰1,王栋芳1,曹 冰1,罗世恒2,刘雅琼1,黄宁华1,闫赖赖1,王京宇1*. GC-MS测定血清胆固醇及其标志物前处理条件正交试验优化研究[J]. 光谱学与光谱分析, 2016, 36(05): 1488-1493.
ZHANG Yu1, WANG Dong-fang1, CAO Bing1, LUO Shi-heng2, LIU Ya-qiong1, HUANG Ning-hua1, YAN Lai-lai1, WANG Jing-yu1*. Orthogonal Experiment for Optimization of the Sample Pretreatment Conditions for the Serum Cholesterol and Markers Determination by GC-MS. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2016, 36(05): 1488-1493.
[1] Gylling H. International Journal of Clinical Practice, 2004, 58(9): 859. [2] Mia Hedman, Miettinen Tatu A, Gylling Helena, et al. The Journal of Pediatrics, 2006, 148(2): 241. [3] Miettinena Tatu A, Gylling Helena, Viikari Jorma, et al. Atherosclerosis, 2008, 200(1): 177. [4] Silbernagel Guenther, Fauler Guenter, Renner Wilfried, et al. Journal of Lipid Research, 2009, 50(2): 334. [5] Miettinen T A, Gylling H, Nissinen M J. Nutrition, Metabolism and Cardiovascular Diseases, 2011, 21(10): 765. [6] Edwards Selvin H, Kimberly Mary M, Pyatt Susan D, et al. Clinical Chemistry, 2011, 57(4): 614. [7] Zhou W, Li H, Dong J, et al. Clinical Chemistry and Laboratory Medicine, 2011, 49(4): 669. [8] Hojo Kazuhiro, Hakamata Hideki, Takahashi A, et al. Journal of Chromatography B, 2011, 879(11-12): 751. [9] Briche Céline S J Wolff, Carter David, Webb Kenneth S. Rapid Communications in Mass Spectrometry, 2002, 16(9): 848. [10] ZHANG De-ting, FANG Shen-hui, PAN Li-qin, et al(张德亭, 方深慧, 潘利琴, 等). Chinese Journal of Health Laboratory Technology(中国卫生检验), 2014, 24(6): 838. [11] WANG Fang-jie, GUO Cheng-xian, XIAO Shan, et al(王方杰, 郭成贤, 肖 珊, 等). Chinese Pharmaceutical Journal(中国药学), 2012, 47(7): 560. [12] Amaral C, Gallardo E, Rodrigues R, et al. Journal of Chromatography B, 2010, 878(23): 2130. [13] CAI Pin-pin,LU Hong-mei (蔡品品, 卢红梅). Chinese Journal of Analytical Chemistry(分析化学), 2013, 41(8): 1183.