人离体肝组织胺类产生与死亡时间和环境温度的关系

目的探讨在不同环境温度下,人离体肝组织中有机胺类产生量随死亡时间变化的规律,为某些碎尸案的死亡时间推断提供参考资料。方法应用高效液相色谱仪外标法,动态检测人离体肝组织中组胺、腐胺、尸胺和未腐败氨基酸含量。结果在8℃、15℃、23℃和32℃环境下,有机胺类产生量分别于人死后肝脏即刻离体69h、54h、40h和33h趋于最大值,并且在到达峰值之前,各温度组离体肝组织中有机胺类生成量均与死亡时间成正比关系。结论人离体肝组织中有机胺类产生量与死亡时间和环境温度在一定范围内均呈正相关。     

High performance liquid chromatographic determination of alcohols with reference to body distribution of methanol

A method has been developed on reverse phase high performance liquid chromatography for simultaneous determination of methyl, ethyl and isopropyl alcohols under refractive index detection using pure water as the mobile phase. A good separation has been achieved between these alcohols. Detector response was linear with a detection limit of 5 mg/100 ml. Recovery studies were performed by adding known amounts of methyl and ethyl alcohols to blood, lung and liver within the range 80–90%. The reproducibility of the results was always >90%. The quantitative distribution of methyl alcohol in postmortem body tissues and fluids has been reported in three cases of poisoning.     

HPLC测定白芍配方颗粒中芍药苷的含量

目的:测定白芍配方颗粒中芍药苷的含量。方法:以乙腈-1.0 m l/L H3PO4(14∶86)为流动相,采用高效液相色谱法测定白芍配方颗粒中芍药苷的含量,测定波长为230 nm。结果:芍药苷在34.9~450.0μg/m l浓度范围内呈良好的线性关系,r=0.999 5;平均加样回收率为99.8%。结论:HPLC法简便、准确、灵敏度高、重复性好,可以作为白芍配方颗粒的质量控制手段。     

绵羊血浆阿维菌素荧光高效液相色谱检测法的建立

建立了一种绵羊血浆中阿维菌素 (AVM )荧光高效液相色谱 (HPLC)检测法。用甲醇提取绵羊血浆中的AVM ,并用ODS C18固相萃取法进行纯化 ,纯化后的AVM经干燥处理后 ,用三氟乙酸酐和N 甲基咪唑对其进行荧光衍生化 ,用荧光HPLC进行检测。本方法的最低检测限为 0 .1ng/mL ,在血浆AVM含量 2 .5～ 5 0 .0ng/mL范围内 ,标准曲线方程为Y =2 72 12x -10 412 (r =0 .9995 ) ,样品的平均回收率为 92 .0 2 %± 6.3 3 %。批内变异系数 1.98%～ 6.2 2 % ,批间变异系数 2 .3 1%～ 8.94%。检测结果显示 ,本方法灵敏度高 ,干扰少 ,重复性好。     

8例利多卡因过敏性休克死的血药浓度分析

目的研究利多卡因过敏性休克死者利多卡因血药浓度及其与死因的关系。方法采用高效液相色谱法(HPLC),分别对使用利多卡因麻醉术中各项指标均正常的8例术中因利多卡因过敏性休克死者的血液和11例顺利完成手术患者的血液进行利多卡因浓度的检测,对比分析两者结果。结果 8例死者利多卡因血药浓度(1．61mg± 0．45mg／L)低于11例正常患者利多卡因血药浓度(2．44mg±0．47mg／L)。结论利多卡因过敏性休克死者血药浓度在正常值范围内,与发生过敏性休克致死无关。     

乌头属植物生物碱高效液相色谱研究

目的建立高效液相色谱法测定多种乌头属植物生物碱的方法。方法XTerraTMRP185μm,(250mm×4.6mm)色谱柱;流动相为乙腈∶30mmol/L碳酸氢铵梯度洗脱;流速1.0ml/min;检测波长233nm。结果该方法可成功应用于5种乌头属植物12个样品中生物碱成分分析。结论本研究结果提示乌头属不同种植物中生物碱成分及含量差异显著,因此为确保该类中药材用药安全,提高临床疗效,必须建立严格的药材质量控制体系。     

Determination of MDMA, MDA, MDEA and MBDB in oral fluid using high performance liquid chromatography with native fluorescence detection

This paper describes the analytical methodology for the determination of MDMA, MDA, MDEA and MBDB in oral fluid. After a liquid–liquid extraction, the analysis was carried out by high performance liquid chromatography (HPLC), with fluorescence detection. The detector wavelength was fixed at 285 nm for excitation and 320 nm for emission. The mobile phase, a mixture of phosphate buffer (pH = 5) and acetonitrile (75:25), and the column, Kromasil 100 C8 5 μm 250 mm × 4.6 mm, allowed good separation of the compounds in an isocratic mode in only 10 min. The method was validated and showed good limits of detection (2 ng/mL) and quantitation (10 ng/mL) for all the amphetamine derivatives. No interfering substances were detected. A stability study of these compounds in oral fluid stored at three different temperatures (−18, 4 and 20 °C) over 10 weeks was conducted, showing a time-dependent degradation of the four compounds.     

高效液相色谱法测定肝组织中4种蟾蜍二烯内酯类化合物

目的建立高效液相色谱法检测肝组织中蟾蜍二烯内酯的定量方法。方法 以OasisHLB固相萃取柱对样品进行提取,应用HPLC色谱法分离、二极管阵列检测器测定。结果该方法的回收率高于70％,线形范围在12ng/g-1200ng/g,经该方法测得华蟾毒它灵、蟾毒灵的最小检出量为O.4ng,华蟾毒精、脂蟾毒配基的最小检出量为0.5ng(S/N≥3)。结论该方法快速、灵敏、准确,可用于蟾酥中毒的法医学检验。     

HPLC测定杞菊地黄胶囊中马钱苷的含量

目的:建立高效液相色谱法测定杞菊地黄胶囊中马钱苷的含量。方法:以十八烷基硅烷键合硅胶为填充剂,流动相为乙腈∶水(15∶85),检测波长为236 nm,柱温25℃,理论板数按马钱苷峰面积计算不低于4 000。结果:马钱苷量在12.04-120.40μg/L范围内具有良好线性关系,A=14.189c-21.25,r=0.999 4,平均加样回收率为105.58%。结论:该方法方便、快捷、准确,灵敏度高,重现性好。     

损伤皮肤中白三烯B_4含量测定与损伤时间推断

本文作者利用高压液相色谱,快速检测大鼠皮肤切创创缘组织中白三烯B_4含量。结果发现,生前各损伤时间组创缘中白三烯B_4含量明显升高,且在1小时内与损伤时间有一定线性关系;死后损伤标本未见白三烯B_4含量升高。由此表明白三烯B_4含量测定,对推断生前1小时内的损伤时间有重要价值。高压液相色谱能快速、准确地检测损伤组织中的白三烯B_4。