GC-MS法测定尿中γ-羟基丁酸  

Determination of γ-hydroxybutyric acid in urine by GC-MS

作　　者：张绍雨[1] 林云珠[2] 柯洪伟[2] 彭亦如[2] 黄增萍[3] 

机构地区：[1]福建公安高等专科学校,福州350007 [2]福建师范大学化学与材料学院,福州350007 [3]福建省公安厅刑警总队,福州350003

出　　处：《分析仪器》2005年第2期24-27,共4页Analytical Instrumentation

摘　　要：γ-羟基丁酸(GHB)是娱乐场所滥用的麻醉药。本文用气相色谱-质谱法(GC -MS)测定尿中GHB。尿样酸化后于80℃经2 0minGHB转化为丁内酯(GBL) ,用二氯甲烷提取,气相色谱质谱 选择离子检测模式测定,正己酸为内标。检测离子GBL为m z 86、5 6、4 2、2 8,内标为m z 87、73、6 0、4 1,定量离分别为m z 86和87。方法检出限0 .0 8μg mL(S/ N =3)。尿中加标10 μg mL ,6次测定的相对标准偏差为2 .5 % ,回收率5 7.7%。线性范围0～5 0μg mL,相关系数(r2 )为0 .9996。用该方法分析2 0个尿样,GHB浓度都低于1μg mL。该方法灵敏度高,简单可靠,适用于法医和临床检验。hydroxybutyric acid (GHB) is a drug abused in creational places. A method for the determination of GHB in urine by GC-MS is described. Samples were acidified and GHB was converted to γ-butyrolactone (GBL) at 80℃for 20 min. GBL was extracted with dichloromethane and determined by GC-MS with selected ion monitoring mode using caproic acid as internal standard (IS). The ions monitored were m/z 86, 56, 42 and 28 for GBL and m/z 87, 73, 60 and 41 for IS. The ions for quantitation were m/z 86 and 87 for GBL and IS, respectively. Detection limit was 0.08μg/mL (S/N=3). With 10 μg/mL IS added into urine sample, the RSD was 2.5% (n=6) and the recovery was 57.7%. The linearity was observed in the range of 0～50 μg/mL and r2=0.9996. Twenty urine samples were analyzed (GHB concentrations lower than 1 μg/mL). The method is sensitive, simple and reliable, and is suitable for forensic and clinical tests.

关 键 词：羟基丁酸 测定 MS法 气相色谱-质谱法 GC 相对标准偏差 方法检出限 娱乐场所 二氯甲烷 检测模式 线性范围 相关系数 临床检验 麻醉药 丁内酯 正己酸 回收率 灵敏度 尿样 离子 内标 

分 类 号：R115[医药卫生—公共卫生与预防医学]