药物中的残留溶剂

目的介绍药物中的残留溶剂。方法对ICH、欧洲药典、美国药典和中国药典有关残留溶剂等问题进行讨论。结果与结论对药物中的残留溶剂应引起重视并应规定其允许残留量。第3类溶剂的残留量可用干燥失重法测定，而大多数第1类和第2类溶剂的残留量则用顶空气相色谱法测定。     

超临界流体萃取柴胡果实精油及其化学成分分析

目的:提取柴胡果实精油并分析其化学组成.方法:采用超临界流体革取技术(Supercritical Fluid Extraction,简称SFE)提取柴胡果实的精油,气相色谱-质谱联用仪(GC-MS)分析和鉴定其化学成分.结果:精油的提取率为6.60%(V/W),确定了73个化合物.结论:首次采用超临界革取法从柴胡果实中提取精油,精油的提取率是柴胡根的3倍多,亚油酸、鲸蜡醇乙酸酯、亚油酸乙酯、(-)石竹烯氧化物的相对含量分别为34.85%、16.63%、2.64%、1.81%,植醇、鲸蜡醇乙酸酯、亚油酸乙酯、(-)-石竹烯氧化物为首次从该属植物中发现.     

GC测定痛瘀消散贴中冰片和樟脑的含量

目的:采用GC测定痛瘀消散贴中冰片和樟脑的含量.方法:石英毛细管色谱柱(30m×0.28mm,0.32μm,聚甲基硅油,HP-5),FID检测器,检测温度250℃,进样口温度200℃,分流比10.0:1.结果:冰片以龙脑计,龙脑在0.0897～0.5384μg范围内,龙脑与内标物的峰面积比值呈良好线性关系(r=0.9999,n=6),平均回收率为96.47%;樟脑在0.0950～0.5702μg范围内,樟脑与内标物的峰面积比值呈良好线性关系(r=0.9999,n=6),平均回收率为1 00.02%.结论:该方法简单、快速、准确,可用于该制剂的质量控制.     

Supercritical fluid extraction of essential oil from the fruits of Bupleurum chinense DC. and their characterization by GC/MS

IntroductionChaihuhasbeenusedasoneofthecommontraditionalchinesemedicinesandisoftenemployedtotreatcoldswithfever,alternatingchillsandfever,feelingoffullnessandchestoppression,andhypochondriasis[1 ] .Itssaikopaponins ,essentialoilhavebeenwellinvestigated .10ursane typetriterpeneglyco sides,19oleanane typetriterpeneglycosidesfromthefruitsofBupleurumrotundifoliumhavebeenisolated ,inaddition ,ursane typetriterpeneglycosideswereshowedtopossessantiprolifera tiveactivity[2 ] .Toourknowledge ,thechemic…     

Automated solid-phase extraction and two-step derivatisation for simultaneous analysis of basic illicit drugs in serum by GC/MS

A combination of automated solid-phase extraction (SPE) and subsequent two-step derivatisation has been developed for the simultaneous analysis of basic drugs of abuse and cocaine metabolites in serum samples. Substances included in this procedure are morphine, codeine, methadone, cocaine, benzoylecgonine, methylecgonine, amphetamine, methamphetamine, MDMA, MDEA and MDA. SPE with mixed-mode cartridges (RP-C8 and cation-exchange) was fully automated with a Zymark RapidTrace SPE robot. GC/MS analysis was performed after derivatisation with a new two-step reaction by trifluoroacetic anhydride and 2,2,3,3,3-pentafluoropropanol. High recoveries (> 85%) with high reproducibility (CV 1.1-3.8%) were found for all drugs. High correlation coefficients (r > 0.998) were obtained due to the addition of deuterated standards prior to extraction. Experience obtained over 2 years of applying this method to drug analysis in serum is discussed.     

石菖蒲挥发油的气相色谱指纹图谱研究

目的:建立石菖蒲挥发油的气相指纹图谱,以控制其质量。方法:进样口温度为250℃,检测器温度为280℃,载气为氮气, 流速为1．3ml／min,并采用程序升温对10批石菖蒲中挥发油成分的气相色谱进行分析。结果:共标出6个特征峰,其平均峰面积之 和为总峰面积的(75．4±13．7)％。结论:本方法精密度、重现性、稳定性好,各挥发油成分分离较好,所建立的指纹图谱可作为石菖 蒲的质量控制依据。     

细辛脑中有机溶剂残留的固体顶空毛细管GC测定

建立了固体顶空毛细管气相色谱法测定细辛脑中有机溶剂残留量.采用DB-1大口径毛细管柱,以正丙醇为内标.甲醇、乙醇、二氯甲烷、正己烷、甲苯的回收率分别为102.5%、103.7%、96.1%、91.4%和92.9%,检测限分别为0.02、0.02、0.02、0.01和0.02μg/g.     

乙酸奥曲肽中有机溶剂残留量的毛细管GC测定

建立了毛细管气相色谱法测定乙酸奥曲肽中有机溶剂乙醚、甲醇、二氯甲烷、N,N-二甲基甲酰胺的含量.用HP-Innowax毛细管柱,程序升温的方法.各组分的线性范围分别为25～300、25～300、15～180和25～300μg/ml(r均大于0.999).平均回收率分别为99.7%、99.5%、99.3%和99.2%.检测限分别为1、1、0.6和1ng.