论文部分内容阅读
目的:建立固相萃取-气质联用并结合同位素峰形检索技术(SPE-GC/MS-CLIPS)分析钩吻中的钩吻碱和钩吻碱子的方法。方法:样品采用1%盐酸超声提取,经PCX固相萃取小柱净化,再用氨化甲醇进行洗脱,洗脱液浓缩后用丙酮定容。供试液通过气相色谱质谱联用仪结合毛细管柱(HP-5MS 0.25 mm×30 m×0.25μm),用全扫描模式(m/z 40~500)采集数据后,利用同位素-C峰形检索技术对目标峰进行校正分析。结果:根据钩吻植物的生物碱提取物所得到的质谱谱图,通过与NIST标准库的匹配与同位素峰形检索技术推算的分子式,确定了钩吻中的钩吻碱和钩吻碱子。该方法成功应用于钩吻中毒司法鉴定案例2例,共10批样品。结论:固相萃取-气质联用结合同位素峰形校正检索技术可以准确分析钩吻中的钩吻碱和钩吻碱子,能应用于钩吻的植物鉴定和钩吻中毒司法鉴定工作。
OBJECTIVE: To establish a method for the determination of garnose and kallikin in kyphus kyphus by solid-phase extraction coupled with gas chromatography-mass spectrometry (SPE-GC / MS-CLIPS). Methods: The samples were extracted with 1% hydrochloric acid by ultrasonic extraction, purified by PCX solid phase extraction cartridges, and then eluted with ammoniated methanol. The eluate was concentrated and then fixed with acetone. The test solution was collected by GC-MS with a capillary column (HP-5MS 0.25 mm × 30 m × 0.25 μm) and data was acquired by full scan mode (m / z 40-500) Technology to correct the target peak analysis. Results: According to the mass spectrogram obtained from the alkaloid extract of hook-kinked plants, the formulas of hook-kisel and hook-kisel were determined by the formulas deduced from the match with NIST standard library and the technique of isotopic peak shape retrieval. The method has been successfully applied to kissing poisoning forensic cases of 2 cases, a total of 10 batches of samples. CONCLUSIONS: Solid phase extraction coupled with gas chromatography-mass spectrometry (GC-MS / MS) and isotope peak shape correction (FPSA) technique can accurately analyze the nitidine and kojic konjacs in kyphosis and can be used in identification of kyphosis and forensic identification of kyphosis.