Wu Chen N B, Schaffer M I, Lin R L, Kurland M L, Donoghue E R, Stein R J
J Forensic Sci. 1983 Apr;28(2):398-403.
A general toxicology unknown case is presented to demonstrate our systematic approach. A 20-year-old male was found dead with multiple suicide notes. Overdose was suspected but substances were not known. Blood alcohol was negative. Urine was analyzed by enzyme-multiplied immunoassay technique and was negative for all drugs assayed. Urine was then extracted with ethyl acetate:hexane (1:1) at pH 10 and back-extracted into 1.0N sulfuric acid. The acidic layer was adjusted to pH 10, and re-extracted with ethyl acetate:hexane (1:1). The residue was analyzed by gas chromatography (GC) on a 3% OV-101 column. It was found to be negative for all commonly screened substances. However, several unknown peaks were observed. Electron impact mass spectra of these unknown peaks were obtained and searched for in our computer library of more than 25000 mass spectra. These unknown peaks were identified as doxylamine and pyrilamine by gas chromatography/mass spectrometry. The base peak and molecular ion for pyrilamine were at m/z 121 and 285, respectively. The base peak for doxylamine was at m/z 58. No molecular ion was observed for doxylamine. Both doxylamine and pyrilamine are antihistamines, but are promoted and used in the management of insomnia. Quantitation was performed on a GC using dexbrompheniramine as an internal standard. Blood concentrations for doxylamine and pyrilamine were 0.7 and 7.0 mg/L, respectively. Concentrations in other tissues were determined. Death was caused by combined doxylamine and pyrilamine intoxication; the manner of death was suicide.
本文介绍了一个一般毒理学未知案例，以展示我们的系统方法。一名20岁男性被发现死亡，留有多张自杀遗书。怀疑是过量服药，但具体药物不明。血液酒精检测呈阴性。采用酶增强免疫测定技术对尿液进行分析，所有检测药物均为阴性。然后将尿液在pH 10条件下用乙酸乙酯：己烷（1:1）萃取，并反萃取到1.0N硫酸中。将酸性层调至pH 10，再用乙酸乙酯：己烷（1:1）萃取。残留物在3% OV - 101柱上用气相色谱（GC）分析。结果发现所有常见筛查物质均为阴性。然而，观察到几个未知峰。获取了这些未知峰的电子轰击质谱，并在我们拥有超过25000个质谱的计算机库中进行搜索。通过气相色谱/质谱法将这些未知峰鉴定为多西拉敏和吡苄明。吡苄明的基峰和分子离子分别为m/z 121和285。多西拉敏的基峰为m/z 58。未观察到多西拉敏的分子离子。多西拉敏和吡苄明均为抗组胺药，但也被用于促进和治疗失眠。使用右溴苯那敏作为内标在气相色谱上进行定量分析。多西拉敏和吡苄明的血液浓度分别为0.7和7.0 mg/L。测定了其他组织中的浓度。死亡原因是多西拉敏和吡苄明联合中毒；死亡方式为自杀。
