海桐花蕾挥发油的GC-MS分析

目的:提取海桐花蕾中的挥发性成分。方法:采用固相微萃取法和水蒸气蒸馏法,并用GC-MS测定其化学成分,分别鉴定了67种和41种成分,并用归一化法测定其相对百分含量。结果:与水蒸气蒸馏法相比,固相微萃取法得到的十一烷、壬烷、α-荜澄茄油烯等的含量增加;同时提取出了水蒸气蒸馏法不能蒸馏出来的一些成分,如:α-胡椒烯、α-金合欢烯、β-月桂烯、马鞭草烯等。结论:采用固相微萃取法和水蒸汽蒸馏法,提取挥发油的时间明显缩短     

桂花(晚银桂、贵妃红和窈窕淑女)挥发性成分分析

目的:分析3种桂花的挥发性成分。方法:采用顶空固相微萃取和气质联用技术(HS-SPME-GC-MS),首次分析了桂花花的挥发性成分。结果:从晚银桂、贵妃红和窈窕淑女的花中共鉴定出66种组分。用峰面积归一化法测定了其相对含量,其相对含量分别占总挥发性组分峰面积的79.96%、71.83%和83.61%。结论:首次分析了不同品种桂花的挥发性成分,为进一步开发利用桂花资源提供依据。     

HS-SPME-GC-MS分析河南产牛至挥发性成分

目的：分析牛至的挥发性成分。方法：采用顶空固相微萃取和气质联用技术（HS-SPME-GC-MS）,结合保留指数法并用峰面积归一化法测定相对百分含量。结果：从牛至中鉴定出了30种挥发性成分,占总峰面积的99.59%,其中麝香草酚（43.28%）、麝香草甲醚（11.79%）、石竹烯（11.17%）、2-异丙基甲苯（8.10%）和γ-松油烯（6.37%）等的含量较高。结论：牛至的主要挥发性成分为单萜和倍半萜类。     

海桐花挥发油的提取工艺研究

目的比较固相微萃取法和水蒸气蒸馏法提取海桐花中的挥发性成分差异。方法采用GC-MS测定其化学成分。结果分别鉴定了62种和58种成分。结论与水蒸气蒸馏法相比,固相微萃取法得到的十一烷、壬烷等烷烃的含量增加;并且提取出了水蒸气蒸馏法不能蒸馏出来的一些成分,如马鞭草烯醇、γ-榄香烯、白菖烯、(-)-α-古芸烯、绿花白千层醇等。     

顶空固相微萃取-GC-MS法分析鸡胚地龙膏中挥发性成分

目的:检测鸡胚地龙膏中的挥发性成分。方法:采用顶空固相微萃取法提取样品,用气相色谱-质谱联用技术对鸡胚地龙膏的挥发性成分进行分析。结果:鸡胚地龙膏的主要挥发性组分为烷烃类、萜烯类和酯类化合物,含量较高的为己烷、1,2,3-丙三醇二乙酸酯和2,6-二叔丁基-4-甲基酚。温度为60℃时萃取效果较好。结论:本试验结果可为鸡胚地龙膏治疗急性软组织损伤的临床应用及机制研究提供依据。     

白鲜皮挥发油成分的SPME-GC-MS分析

目的分析白鲜皮挥发油成分。方法利用固相微萃取/气相色谱/质谱(SPME/GC/MS)联用技术对白鲜皮的挥发油成分进行了研究。结果共鉴定出94种成分,占挥发油总成分的96.82%。结论白鲜皮挥发油主要化学成分是白菖油烯(27.17%)、芳脑醇(11.97%)、反-石竹烯(8.07%)、β-马榄烯(8.04%)、(-)-(a)-古芸烯(6.04%)等。     

Determination of ochratoxin A in human urine by solid-phase microextraction coupled with liquid chromatography-fluorescence detection

A new method for the determination of ochratoxin A (OTA) in human urine samples has been developed using solid-phase microextraction (SPME) interfaced with liquid chromatography-fluorescence detection (LC-FD). This method is simpler and cheaper compared to the most widely adopted clean-up procedures for OTA extraction from urine (usually based on immunoaffinity columns). Briefly, urine samples, diluted 1:5 with phosphate buffer (10 mM, pH 3), were partitioned against chloroform and the aqueous phase extracted by a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber. The fiber was then "statically" desorbed, through a SPME interface, into a LC system operating in isocratic conditions. The linear range investigated in urine was 0.01-1 ng/ml. Within-day R.S.D.% in urine spiked at 0.1 and 1 ng/ml were 3.9 and 1.9, respectively, whereas the between-days R.S.D.% were 5.5 and 3.0, respectively. The limits of detection (LOD) and quantitation (LOQ) calculated at a signal-to-noise ratio of 3 and 10 (noise calculated peak to peak on a blank chromatogram at the OTA retention time) were 0.01 and 0.05 ng/ml, respectively.     

Identification of volatile degradants in formulations containing sesame oil using SPME/GC/MS

Solid-phase microextraction (SPME), in combination with gas chromatography/mass spectrometry (GC/MS), was used to identify an unknown degradant observed during stability studies of a pharmaceutical formulation containing sesame oil. SPME is a solvent-less, rapid, sensitive, and inexpensive extraction method that minimizes sample preparation. SPME combined with GC is a widely used technique in certain fields, such as food, environmental analysis, forensics, and consumer products, but has only rarely been used for the analysis of pharmaceutical formulations. Hexanal, octanal, 2-octenal, 2-decenal, 2-undecenal, and 2,4-decadienal can be detected and identified by GC/MS, but they cannot be detected by LC/MS due to their volatility and low ionization efficiency under atmospheric pressure ionization conditions. Combining the MS data from the GC/MS with LC/DAD data resulted in the identification of the unknown degradant in the formulation as 2,4-decadienal. The presence of this and other aldehydes was attributed to the oxidative degradation of the unsaturated fatty-acid component in vegetable oils.     

西府海棠挥发性成分研究

目的分析西府海棠花的挥发性成分。方法采用顶空固相微萃取和气质联用技术（HS-SPME-GC-MS）进行分析。结果从西府海棠花中鉴定了47种组分,用峰面积归一化法测定,其相对含量占总挥发性组分峰面积的91.71%。结论首次分析了西府海棠花的挥发性成分,指出西府海棠花的潜在药用价值和赋香成分,为进一步开发利用西府海棠资源提供了依据。     

固相微萃取技术及其在药物分析领域中的应用

固相微萃取是基于萃取涂层与样品之间的吸附／吸收-解吸平衡而建立起来的集进样、萃取、浓缩功能于一体的新技术。本文评述了固相微萃取技术的装置、工作原理、操作方法、影响因素及优缺点，介绍了SPME技术在药物分析中的应用近况，并且展望了这一技术的应用前景。