摘要
提出了小体积液相萃取-气相色谱质谱法测定唾液中鸦片类毒品含量的方法。在pH9的磷酸盐缓冲溶液中,1 mL的唾液试样(其中加入乙基吗啡为内标)用150μL的氯仿进行超声提取10min,使吗啡、6-单乙酰吗啡和可待因进入有机相,离心分离,取上清液80μL加入N-甲基-双-三氟乙酰胺试剂进行衍生化,所得衍生化产物的溶液做气相色谱-质谱法检测。唾液中吗啡、6-单乙酰吗啡、可待因的检出限(3S/N)分别为0.005,0.003,0.002mg·L^(-1),标准曲线线性范围均为0.01～1.0mg·L^(-1)。在唾液试样中添加0.01,0.10,1.00mg·L^(-1)L混合标准溶液,测得平均回收率:吗啡为38.1%～50.0%,6-单乙酰吗啡为81.5%～88.8%,可待因为89.9%～109.8%,相对标准偏差(n=5)在6.7%～18.4%之间。
Opiates（i.e.,morphine,6-monoacetylmorphine and codeine）in saliva were determined by GC-MS with small volume liquid extraction.In a phosphate buffer solution of pH 9.1 mL of soliva sample was extracted ultrasonically with 150μL of chloroform for 10 min.After centrifugation.80μL of the supernatant liquid was taken and derivatized with the reagent N-methyl-bis-trifluoroacetamide,and the derivitized product in the solution was determined by GC-MS.Values of detection limit（3S/N）found for the 3 opiates mentioned above were 0.005, 0.003.0.002 mg·L^-1respectively.Ethyl morphine was used as internal standard.Ranges of linearity of calibration curves for the 3 opiates were same in the range of 0.01-1.0 mg·L^-1,Recovery and precision of the method were tested by addition of mixed opiate standard at 3 concentration levels,giving values of recovery in the ranges of 38.1%-50.0%（for morphine）,81.5%-88.8%（for 6-monoacetylmorphine）and 89.9%-109.8% （for codeine）;with values of RSD＇s（n=5）in the range of 6.7%-18.4%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2011年第4期442-444,448,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家"十一五"支撑项目(2006BAK09B06)
北京教育委员会共建项目建设计划(SYS 1004100436)
