GC-MS法同时检测人尿液中10种常见安眠药物  被引量:4

Simultaneous Determination of 10 Kinds of Common Hypnagogues in Human Urine by GC-MS

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作  者:袁烨[1] 郭巍巍[1] 李军[1] 于天晓[1] 杨硕[1] 

机构地区:[1]河北省儿童医院儿科研究所,石家庄050011

出  处:《中国药房》2013年第46期4362-4364,共3页China Pharmacy

摘  要:目的:建立同时检测人尿液中10种常见安眠药物的方法。方法:采用乙醚提取,气-质联用(GC—MS)法检测。系统地对体系pH值、提取时间等样品预处理条件以及色谱柱等GC—MS分析条件进行考察优化。运用选择离子模式(SIM)进行检测,每种成分选择2~3个特征离子。所选离子分别为:巴比妥m/z 156、141(定量离子)、185,苯巴比妥m/z 204(定量离子)、117,异戊巴比妥m/z 156(定量离子)、141、227,司可巴比妥m/z 168(定量离子)、195、239,地西泮m/z 256(定量离子)、283,硝西泮m/z 264、280(定量离子),阿普唑仑m/z 273、308(定量离子),咪达唑仑m/z 310(定量离子)、325,氯丙嗪m/z 58(定量离子)、318,氯氮平m/z 326、256(定量离子)。结果:在选定的试验条件下,10种安眠药物在相应范围内线性关系良好,方法回收率在92.6%~97.3%之间,RSD在2.46%~5.19%之间,检出限为0.02~0.30gg/ml。结论:本法简便、快速、灵敏、可靠,可应用于患者尿液样品中药物成分的分析检测。OBJECTIVE: To develop a method for simultaneous determination of 10 kinds of hypnagogues in human urine. METHODS: Drugs were extracted with ethyl ether and detected by GC-MS. The effects of pH and the extraction time were studied and the GC operating conditions were optimized. GC-MS selective ion monitoring (SIM) mode was used to detect the 2-3 characteristic ions. The characteristic ions were: barbital m/z 156, 141 (quantitative ion) and 185; phenobarbitone m/z 204 (quantitative ion), 117; amobarbital m/z 156 (quantitative ion), 141 and 227; secobarbital m/z 168 (quantitative ion), 195 and 239; diazepam m/z 256 (quantitative ion), 283; nitrazepam m/z 264, 280 (quantitative ion) ; alprazolam m/z 273, 308 (quantitative ion) ; midazolam m/z 310 (quantitative ion), 325; chlorpromazine m/z 58 (quantitative ion), 318; clozapine m/z 326, 256 (quantitative ion). RESULTS: A good linearity of 10 kinds of hypnagogues was obtained at the corresponding concentration range. The recoveries were between 92.6%-97.3%, and the relative RSD were between 2.64%-5.19 %. The detection limits were 0.02-0.30 μg/ml. CONCLUSIONS: The method is simple, rapid, sensitive and reliable, and it can be used for the determination of the hypnagogues in human urine.

关 键 词:气-质联用法 尿液 安眠药物 

分 类 号:R969.1[医药卫生—药理学] R971.5[医药卫生—药学]

 

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