光谱学与光谱分析, 2016, 36 (5): 1488, 网络出版: 2016-12-20  

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

Orthogonal Experiment for Optimization of the Sample Pretreatment Conditions for the Serum Cholesterol and Markers Determination by GC-MS
作者单位
1 北京大学公共卫生学院, 北京 100191
2 岛津企业管理(中国)有限公司, 北京 100020
摘要
采用正交试验优化GC-MS测定血清胆固醇及其标志物的样品前处理条件, 并对最优试验方案进行方法学评价。 采用L16(211)正交设计对影响GC-MS测定血清胆固醇及其标志物前处理的3个关键步骤共7个因素——皂化(KOH-乙醇浓度、 皂化温度和时间)、 萃取(正己烷用量)和衍生化(衍生化温度、 时间和用量)进行优化。 得到最优前处理条件组合如下: KOH-乙醇溶液浓度为1 mol·L-1; 皂化温度70 ℃; 皂化时间60 min; 萃取剂用量2 mL; 衍生化温度70 ℃; 衍生化时间60 min; 衍生化试剂用量100 μL。 所建方法准确性和精密性良好, 方法学评价指标优于文献报道。
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, 王栋芳, 曹冰, 罗世恒, 刘雅琼, 黄宁华, 闫赖赖, 王京宇. 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(5): 1488. ZHANG Yu, WANG Dong-fang, CAO Bing, LUO Shi-heng, LIU Ya-qiong, HUANG Ning-hua, YAN Lai-lai, WANG Jing-yu. Orthogonal Experiment for Optimization of the Sample Pretreatment Conditions for the Serum Cholesterol and Markers Determination by GC-MS[J]. Spectroscopy and Spectral Analysis, 2016, 36(5): 1488.

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