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pH 9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150 μL的氯仿进行超声提取10 min,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80 μL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0.005,0.003,0.002 mg·L-1,标准曲线线性范围均为0.01~1.0 mg·L-1。在唾液试样中添加0.01,0.10,1.00 mg·L-1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 150 μL of chloroform for 10 min. After centrifugation, 80 μL 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-1 respectively. 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%.