目的采用液液提取与液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,LC-MS/MS)技术,建立同时测定血液中13种安眠镇静类药物及其代谢产物的分析方法,并将其应用于实际案例。方法血液加入内标后,用乙酸乙酯提取,浓缩...目的采用液液提取与液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,LC-MS/MS)技术,建立同时测定血液中13种安眠镇静类药物及其代谢产物的分析方法,并将其应用于实际案例。方法血液加入内标后,用乙酸乙酯提取,浓缩至近干后,用甲醇溶解残渣,过0.22μm滤膜后测定。13种安眠镇静类药物及其代谢物经C18色谱柱分离,以甲醇和20 mmol/L甲酸铵(含0.1%甲酸)水溶液进行梯度洗脱,电喷雾正离子模式检测,内标法定量。结果血液中13种安眠镇静类药物及其代谢物在5~200μg/L范围内具有良好的线性关系,相关系数为0.990 3~0.999 8,检出限为0.1~1.0μg/L;在10、50、200μg/L3个添加浓度水平的回收率为71.2%~93.4%,日内和日间精密度≤8.6%,准确度(偏倚)在±9.8%范围内。结论本方法快速、简单、高效、灵敏度高,可用于法医毒物学领域血液中13种安眠镇静类药物及其代谢产物的分析。展开更多
Objective To study the hypnotic and anticonvulsant activities of the leaves of Eucommia ulmoides(LEU),the total alkaloids were extracted from LEU using water-acid method.Methods Mice were divided into five groups,in...Objective To study the hypnotic and anticonvulsant activities of the leaves of Eucommia ulmoides(LEU),the total alkaloids were extracted from LEU using water-acid method.Methods Mice were divided into five groups,including groups contained total alkaloids in three different doses,negative and positive control groups.Direct hypnotic experiment in mice,pentobarbital sodium synergistic experiment,and anticonvulsant experiment were used.The numbers of spontaneous activities,sleep rate,sleep latency,sleep time,convulsion rate,and convulsion latency of the mice were recorded and analyzed.Results The total alkaloids from LEU could increase the sleep rate,significantly lengthen the sleep time,and shorten the sleep latency of mice.Even the low dose of total alkaloids(0.33 g/kg)showed significantly different activities with negative control group(physiological saline)with the synergistic effect of the superthreshold dose of pentobarbital sodium.Furthermore,the total alkaloids efficiently inhibited the convulsion caused by nikethamide.Conclusion The total alkaloids from LEU have the excellent sedative,hypnotic,and anticonvulsant activities in mice,with high safety and little drug side effects.Therefore,they have the protential development prospects in sedative-hypnotic drugs.展开更多
基金National Natural Science Foundation of China(31000017)
文摘Objective To study the hypnotic and anticonvulsant activities of the leaves of Eucommia ulmoides(LEU),the total alkaloids were extracted from LEU using water-acid method.Methods Mice were divided into five groups,including groups contained total alkaloids in three different doses,negative and positive control groups.Direct hypnotic experiment in mice,pentobarbital sodium synergistic experiment,and anticonvulsant experiment were used.The numbers of spontaneous activities,sleep rate,sleep latency,sleep time,convulsion rate,and convulsion latency of the mice were recorded and analyzed.Results The total alkaloids from LEU could increase the sleep rate,significantly lengthen the sleep time,and shorten the sleep latency of mice.Even the low dose of total alkaloids(0.33 g/kg)showed significantly different activities with negative control group(physiological saline)with the synergistic effect of the superthreshold dose of pentobarbital sodium.Furthermore,the total alkaloids efficiently inhibited the convulsion caused by nikethamide.Conclusion The total alkaloids from LEU have the excellent sedative,hypnotic,and anticonvulsant activities in mice,with high safety and little drug side effects.Therefore,they have the protential development prospects in sedative-hypnotic drugs.