Simultaneous determination of heroin, 6-monoacetylmorphine, morphine, and its glucuronides by liquid chromatography atmospheric pressure ionspray mass spectrometry
Simultaneous determination of heroin, 6-monoacetylmorphine, morphine, and its glucuronides by liquid chromatography atmospheric pressure ionspray mass spectrometry
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DOI：
10.1093/jat/21.4.268
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发表时间：
1997-07-01
影响因子：
2.5
通讯作者：
DAscenzo, G
中科院分区：
文献类型：
--
作者：
Zuccaro, P;Ricciarello, R;DAscenzo, G
建立了一种新的液相色谱-离子喷雾质谱法同时测定血清中海洛因、6-单乙酰吗啡、吗啡、吗啡-6-和3-葡萄糖醛酸苷和可待因的分析方法。分析物和内标物，纳洛啡，进行固相萃取（SPE），使用乙基SPE色谱柱前。采用正相色谱柱和水-甲醇-乙腈-甲酸移动的相，流速为230 µL/min，质谱仪以选择离子监测模式运行。在这些条件下，海洛因的定量限为0.5 ng/mL，6-单乙酰吗啡为4 ng/mL，吗啡为4 ng/mL，吗啡-3-葡糖苷酸为1 ng/mL，吗啡-6-葡糖苷酸为4 ng/mL，可待因为4 ng/mL。C57 BL/6近交系小鼠皮下注射20 mg/kg海洛因后，测定血清中海洛因代谢产物的水平。6-单乙酰吗啡在3分钟时显示出0.93 µg/mL血清的峰浓度，而吗啡和吗啡-3-葡糖苷酸分别在10和20分钟时达到9.6和2.9 µg/mL血清的峰浓度。最后，吗啡-6-葡糖苷酸和可待因的缺乏排除了在该动物模型中由吗啡形成的可能性。
A new analytical technique has been developed for the simultaneous determination of heroin, 6-monoacetylmorphine, morphine, morphine-6- and 3-glucuronides, and codeine in serum using liquid chromatography coupled with ionspray mass spectrometry. The analytes and the internal standard, nalorphine, were subjected to solid-phase extraction (SPE) using ethyl SPE columns before chromatography. The chromatographic separation of the analytes was achieved using a normal phase column and a water-methanol-acetonitrile-formic acid mobile phase at a flow rate of 230 µL/min. The mass spectrometer was operated in selected-ion monitoring mode. Under these conditions, the limit of quantitation was 0.5 ng/mL for heroin, 4 ng/mL for 6-monoacetylmorphine, 4 ng/mL for morphine, 1 ng/mL for morphine-3-glucuronide, 4 ng/mL for morphine-6-glucuronide, and 4 ng/mL for codeine. Serum levels of heroin metabolites were determined in C57BL/6 inbred mice after a dose of 20 mg/kg heroin administered subcutaneously. 6-Monoacetylmorphine showed a peak concentration of 0.93 µg/mL serum at 3 min, whereas morphine and morphine-3-glucuronide achieved their peak concentrations of 9.6 and 2.9 µg/mL serum at 10 and 20 min, respectively. Finally, the absence of morphine-6-glucuronide and codeine excluded the possibility of their formation from morphine in this animal model.