在pH 9的磷酸盐缓冲介质中,人血试样(其中加乙基吗啡为内标)用氯仿、异丙醇及正庚烷(50+17+33)的混合溶剂进行超声萃取10 min,使其中吗啡、6-单乙酰吗啡和可待因进入有机相.离心分离,取上清液常温下吹干.残渣溶于乙酸乙酯中并用MBTFA试剂进行衍生化,取经衍生化的溶液1 μL作气相色谱-质谱测定.人体血液中吗啡、6-单乙酰吗啡、可待因的检出限(3S/N)分别为1,2,3 μg·L-1,标准曲线线性范围均为10~1 000 μg·L-1.1 mL血液中添加10,100,1 000 ng 3个浓度药物,平均相对回收率吗啡为82.4%~85.5%,6-单乙酰吗啡为95.7%~99.1%,可待因为97.5%~101.2%.相对标准偏差(RSD,n=5),RSD日内为4.1%~11.2%,RSD日间为4.9%~12.1%.

In a phosphate buffer of pH 9,opiates (i.e.,morphine,6-monoacetylmorphine and codeine) in human blood sample were extracted ultrasonically with a mixture of chloroform,iso-propanol and n-heptane(50+17+33 by volume) at 30 ℃ for 10 min. After centrifugation,the supernatant liquid was taken and evaporated to dryness by blowing at room temperature. The residue was dissolved with acetylacetate and derivatized with the reagent MBTFA. An aliquot of 1 μL of the derivitized solution was taken for GC-MS determination. Values of DL (3S/N) found for the 3 opiates mentioned above were 1,2 and 3 μg·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 10-1 000 μg·L-1. Recovery and precision of the method were tested by addition of the opiate standards at 3 different concentration levels,giving values of recovery in the ranges of 82.4%-85.5% (for morphine),95.7%-99.1% (for 6-monoacetylmorphine) and 97.5%-101.2% (for codeine);and values of RSD′s (n=5) in the ranges of 4.1%-11.2% (within day) and 4.9%-12.1% (inter day).