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：张钰[1] 王栋芳[1] 曹冰[1] 罗世恒 刘雅琼[1] 黄宁华[1] 闫赖赖[1] 王京宇[1] 

机构地区：[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

出　　处：《光谱学与光谱分析》2016年第5期1488-1493,共6页Spectroscopy and Spectral Analysis

基　　金：北京大学医学交叉学科种子基金项目(BMU20140435)资助

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L_(16)(2^(11))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1mol·L^(-1);皂化温度70℃;皂化时间60min;萃取剂用量2mL;衍生化温度70℃;衍生化时间60min;衍生化试剂用量100μL。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。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 L_（16）（2^（11））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 60min;the Solvent quantity is 2mL;the derivatization temperature is 70 ℃;the derivatization time is 60 min,and the derivatization agent is 100μL.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.

关 键 词：GC-MS 正交试验 胆固醇 标志物 前处理 

分 类 号：R113[医药卫生—公共卫生与预防医学]