顶空固相微萃取法与水蒸气蒸馏法联合气相色谱-质谱分析肿节风挥发性成分

目的：比较顶空固相微萃取法（HS-SPME）与水蒸气蒸馏法（SD）提取肿节风中挥发性成分的差异。方法：采用气相色谱-质谱（GC-MS）联用技术分析肿节风挥发性成分。结果：采用HS-SPME-GC-MS共分离出59个色谱峰,鉴定出40个化合物,占总挥发性成分的88.47%;SD-GC-MS共分离出59个色谱峰,鉴别出38个化合物,占总挥发性成分的90.04%;2种不同前处理技术共同鉴定出的挥发性成分有11种。结论：HS-SPME与SD联合GC-MS适用于分析不同类型挥发性化学成分,将两种方法联用分析肿节风挥发性成分能够得到更加全面的信息。     

固相微萃取法与水蒸气蒸馏法提取蜘蛛香挥发油成分的比较

目的:比较固相微萃取法与水蒸气蒸馏法提取蜘蛛香挥发油成分的差异。方法:采用气相色谱-质谱联用技术分别对水蒸气蒸馏法和固相微萃取法提取蜘蛛香根茎所得挥发油的化学成分进行比较分析。结果:2种提取方法所得挥发油成分差异较大。与水蒸气蒸馏法比较,固相微萃取法所得挥发油成分数目和种类较多。结论:固相微萃取法比水蒸气蒸馏法具有明显的优越性。     

气质联用法分析大花红景天顶空固相微萃取与水蒸气蒸馏的挥发性成分

目的：比较顶空-固相微萃取法（HS-SPME）和水蒸气蒸馏法（SD）提取红景天中挥发性成分差异。方法：采用顶空固相微萃取法和水蒸气蒸馏法提取红景天挥发性成分,并用GC-MS联用技术对红景天的挥发性成分进行分析。结果：顶空固相微萃取法鉴定出39种挥发性化学成分,水蒸气蒸馏法鉴定出16种挥发性化学成分,共有成分4种。结论：2种方法鉴定出的挥发性成分及其相对含量上存在一定差异,与水蒸气蒸馏法比较,顶空固相微萃取法所得挥发性成分数目和种类较多,具有更高的检索匹配度和灵敏度,有明显的优越性。     

顶空固相微萃取-气质联用分析海桐中挥发性成分

目的:分析海桐果实中挥发性化学成分的组成。方法:采用顶空固相微萃取(HS-SPME)技术对海桐果实进行萃取,用气相色谱-质谱(GC-MS)法进行分离分析。结果:共分离并鉴定出22种化学成分。萃取物中含量最高的成分是α-蒎烯(72.38%),其次为γ-杜松烯(5.66%)、1-异丙烯基-3-异丙酯苯(5.21%)。结论:首次采用HS-SPME-GC-MS联用技术分析海桐果实中的挥发性成分,为海桐挥发性成分的研究及开发利用提供了科学依据。     

水蒸气蒸馏提取与顶空进样气相色谱-质谱分析吴茱萸挥发性成分

目的分析比较不同采集方法制备的吴茱萸中挥发性成分。方法分别采用水蒸气蒸馏法和顶空加热提取挥发性成分的方法,对其进行气相色谱-质谱(GC-MS)分析。结果两种提取方法无论在成分还是其相对含量方面均存在一定的差异,采用水蒸气蒸馏法可鉴定出16种挥发性化学成分,采用顶空进样技术可鉴定出18种挥发性化学成分,共有成分为8种。结论两种样品采集方法,分别提供了不同沸点吴茱萸挥发物的化学信息;运用这两种方法可建立更全面的吴茱萸挥发性成分GC-MS表征体系。     

枇杷花挥发性成分顶空固相微萃取-GC-MS联用法分析

目的:采用顶空固相微萃取-气相色谱-质谱联用(SPME-GC-MS)法分析鉴定枇杷花挥发性成分,并优化SPME的操作条件。方法:色谱柱为DB-5MS石英弹性毛细管柱(30.0m×250μm×0.25μm),载气为高纯氦气(99.999%),流速为1.0mL.min-1,进样口温度为250℃,电离方式为EI源,电离能量为70eV,质量扫描范围为30~440amu。结果:样品在80℃、用65μm聚二甲基硅氧烷-二乙烯苯(PDMS-DVB)萃取头对枇杷花顶空吸附30min,250℃解吸1min,GC-MS对解析物进行分离鉴定,共获得34个峰,鉴定出29个组分,占总峰面积的97.42%,主要为苯甲醛和4-甲氧基苯甲醛。结论:本方法可用于枇杷花中挥发性成分的快速分析。     

顶空固相微萃取气质联用法分析阿育魏实挥发性成分

目的:利用顶空-固相微萃取(HS-SPME)结合气相色谱-质谱联用技术(GC-MS)分析阿育魏实挥发性化学成分,为其挥发性成分分析提供新方法。方法:实验中以PDMS、CAR/PDMS、PDMS/DVB和DVB/CAR/PDMS为微萃取纤维头,顶空固相微萃取方法提取阿育魏实中挥发性成分,采用GC-MS对挥发性成分进行分离鉴定,面积归一化法确定各成分的相对质量分数,并与传统的水蒸气蒸馏法(HD)提取的挥发性成分进行了比较。结果:DVB/CAR/PDMS萃取纤维有效地萃取阿育魏实挥发性成分,其主要成分为γ-萜品烯(26.21%)、p-伞花烃(23.58%)、百里香酚(20.02%)。结论:HD和HS-SPME 2种分析方法共鉴定出22个挥发性成分,主要挥发性物质组分一致。HS-SPME-GC-MS能快速地获得其组成成分,有利于提取易挥发性化合物,特别是对挥发性单萜类和倍半萜类化合物,可应用于阿育魏实挥发性成分的快速分析及质量控制。     

水蒸气蒸馏与顶空进样GC-MS法分析荜茇挥发性成分

分别采用水蒸气蒸馏法和顶空进样法提取荜芨挥发性成分,经GC-MS分析,结果显示,采用水蒸气蒸馏法和顶空进样技术均可鉴定出荜茇中28个挥发性化学成分,其中有17种共有化合物,但相对含量有差异.本研究采用两种样品采集方法,并提供了荜茇中不同沸点的挥发物的化学信息,从而建立更全面的荜茇挥发性成分GC-MS表征体系.     

超临界二氧化碳萃取法与水蒸气蒸馏法提取缬草油的化学成分比较

摘要目的对不同提取方法提取的缬草油化学成分进行比较研究。方法采用超临界二氧化碳（CO2）萃取法和水蒸气蒸馏法从缬草中提取缬草油,用气相色谱 质谱联用（GC MS）法进行化学成分定性与相对含量的比较。结果共鉴定了118种成分,超临界CO2萃取法提取物共鉴定98种,水蒸气蒸馏法提取鉴定了67种,共有成分47种;超临界CO2萃取所得缬草油的收率约为水蒸气蒸馏收率的1.8倍。结论超临界CO2萃取法是缬草油较好的提取方法。     

顶空固相微萃取-GC/MS法分析长鞭红景天的挥发性成分

目的 鉴定分析长鞭红景天的挥发性成分。方法 采用顶空固相微萃取-气质联用技术对长鞭红景天中的化学成分进行鉴定,并结合峰面积归一法确定各组分的含量。结果 鉴定出64种化学物质,占总峰面积的100%,其中,烷烃类33种,酸类3种,醇类12种,醛类5种,酮类4种,烯烃类4种,酯类3种。结论 将顶空固相微萃取-气质联用技术应用于鉴定长鞭红景天的挥发性成分,可以高效、无损地鉴别出其挥发性成分的组成及相对含量。     

姜黄中总姜黄素纯化方法的比较

目的研究总姜黄素较优的纯化方法.方法采用分光光度法,以总姜黄素的含量为指标,考察了从姜黄中提纯总姜黄素的3种不同方法.结果水杨酸钠法所得样品的含量最高为92.5%,其次为酸碱法74.0%,最低为活性炭法51.2%.结论水杨酸钠法操作简单,提取物纯度较高,为较好的纯化方法.     

GC-MS法比较温莪术挥发油与水煎液中的挥发性成分

目的利用GC-MS法比较温莪术传统水煎液与挥发油所含挥发性成分的差别,初步探讨水煎剂中的主要化学成分,为温莪术水煎剂临床疗效物质基础研究积累数据,为温莪术挥发油及其制剂的临床用药给予指导。方法采用GC-MS法对温莪术挥发油和水煎液的乙酸乙酯萃取物化学成分进行分析,通过标准谱库检索结合文献分析,确定温莪术挥发油与水煎液乙酸乙酯萃取物中所含的主要挥发性成分,并对二者所含化学成分进行比较。结果从温莪术挥发油中指认出49种化学成分,从温莪术水煎液乙酸乙酯萃取物中指认出28种化学成分,其中仅有莪术二酮(curdi-one)、斯巴醇(spathulenol)和deoxysericealactone等3种成分为二者共有成分。结论温莪术挥发油与水煎液所含挥发性成分存在显著差别,温莪术水煎液的有效成分需进一步研究。     

顶空固相微萃取-气质联用对滁菊配方颗粒的挥发性成分的分析

目的 分析比较了滁菊以及滁菊配方颗粒的挥发性成分.方法 制备滁菊配方颗粒,并采用顶空固相微萃取结合气相色谱-质谱联用技术对滁菊干花以及滁菊配方颗粒的挥发性成分进行鉴定比对,并用面积归一法测定成分相对含量.结果滁菊干花中共鉴定出40种挥发性化合物,滁菊颗粒中共鉴定出59种挥发性化合物,鉴定了30个共有峰.结论 该方法简单、准确,为滁菊品种配方颗粒提供了一定的鉴别依据.     

超临界CO_2萃取与水蒸气蒸馏法提取太子参挥发油化学成分气质联用研究

目的:分析比较采用超临界CO2流体萃取法与水蒸气蒸馏法提取的太子参提取物中挥发性化学成分的异同。方法:使用水蒸馏提取法和超临界CO2萃取技术从太子参中提取挥发性成分,用归一化法测定其百分含量。用气相色谱-质谱(GC-MS)计算机联用技术分离鉴定其中的化学组成。结果:太子参超临界CO2流体萃取物中初步鉴定了33种成分,主要成分为:亚油酸乙酯(28.70%)、n-十六酸(23.12%)、3-糠醇(5.51%)等;水蒸气蒸馏法提取挥发油初步鉴定了17种成分,主要成分为2-丙基呋喃(22.45%)、3-糠醇(19.78%)、3-乙基-3-甲基戊烷(19.47%)。结论:2种方法提取的挥发油化学成分差异较大,超临界CO2流体萃取法提取的挥发油能更真实、全面地反映太子参药材中的化学成分。     

Determination of lidocaine in hair of drug fatalities by headspace solid-phase microextraction

The local anesthetic lidocaine was determined in hair by hydrolysis of the samples with 4% NaOH in the presence of excessive Na2SO4 and subsequent headspace solid-phase microextraction with a 65-microm Carbowax/divinylbenzene fiber, and gas chromatography-mass spectrometry measurement with etidocaine as the internal standard. The calibration curve was linear between 0.1 and 1000 ng/mg. The detection and quantitation limits were 0.1 and 0.4 ng/mg, respectively. The method was applied to hair samples of 49 drug fatalities, and positive results were obtained in 32 cases with lidocaine concentrations between 0.4 and 400 ng/mg and 675 ng/mg in one extreme case. For comparison, morphine, 6-acetylmorphine, codeine, dihydrocodeine, methadone, cocaine, and benzoylecgonine were also determined by usual methods. From segmental investigations in four of the cases and from comparison with the hair concentrations of the other drugs, it follows that lidocaine was consumed for a longer period of time as an adulterant of cocaine and heroin preparations.     

黔产莪术和种子中提取挥发油的具体成分异同比较

目的研究黔产莪术和莪术种子中挥发油质控成分的检定方法与含量范围。方法建立高效液相色谱法(HPLC)同时测定黔产莪术与莪术种子中吉马酮和呋喃二烯含量方法:色谱柱为C18(4.6 mm×250 mm,5μm),流动相为乙腈(A)-水(B),梯度洗脱(0~20 min,60%A~95%A;20~35 min,95%A),流速为1 ml/min,检测波长为216 nm,柱温35℃,进样量10μl。结果吉马酮和呋喃二烯的检测浓度分别在4.18~83.6μg/m L(r=0.9999),10.21~204.2μg/ml(r=1.0000)范围呈现良好的线性关系;吉马酮和呋喃二烯的平均回收率(n=6)分别103.2%(RSD=1.44%,102.2%(RSD=1.28%),重复性实验(n=6)RSD分别为0.90%,2.10%。结论黔产莪术与莪术种子中提取的挥发油的质量,可以用挥发油中所含吉马酮和呋喃二烯含量进行控制。控制范围是:黔产莪术挥发油中吉马酮,呋喃二烯含量依次是85.87%~100.10%,59.07%~78.92%;黔产莪术种子挥发油中吉马酮,呋喃二烯含量依次是65.69%~80.47%,59.94%~68.41%。     

Determination of volatile organic compounds in biological samples using headspace solid-phase microextraction and gas chromatography: toluene and styrene

Epidemiological and laboratory investigations have shown that toluene and styrene are toxic compounds that lead to impairment of the nervous system. To quantitate toluene and styrene in biological samples, liquid-liquid phase, headspace (HS), and solid-phase microextraction (SPME) methods are generally used. Most of these methods are not sensitive enough for applications involving small sample volumes. Here, we present a method for quantitative analysis of low concentrations of styrene and toluene in very small volumes of biological samples using HS-SPME and gas chromatography (GC) equipped with a flame-ionization detector. The method was developed by optimizing operating parameters that affect the HS-SPME-GC process [i.e., desorption time (30 s), depth of the fiber in the GC injection port (3.7 cm), adsorption time (4 min), and adsorption temperature (room temperature)]. It has a wide range of linearity (0.5-500 ng/10 microL), high precision (coefficient of variation < 5%), good accuracy (deviation < 11%), and low detection limits of 0.13 and 0.08 ng/10 microL for styrene and toluene in serum, respectively. This analytical technique can be applied to the estimation of styrene and toluene in small volumes of biological fluids (blood, serum, and perilymph) and tissues of low lipid content (cochlea).     

Analysis of the volatile compounds of flowers and essential oils from Lavandula angustifolia cultivated in Northeastern Italy by headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry

Headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography and mass spectrometry using the divinyl/carboxen/polydimethylsiloxane (DVB-CAR-PDMS) fibre was applied for the analysis of aroma profiles of Lavandula angustifolia L. flowers and the corresponding essential oils. The optimal sampling time was determined by studying the equilibrium time profile of the major volatile compounds for the lavender flowers (50 min) and the essential oil (20 min). Comparative analysis of L. Angustifolia L. cultivated in Friuli Venezia Giulia (northeastern Italy) highlighted that the contents of linalool and linalyl acetate were the major differences between the composition of flowers and the hydro-distilled products. Lavender essential oil from Middle-Friuli Venezia Giulia was evaluated as the highest quality for its high level of linalyl acetate (31.7 %) and linalool (45.0 %) and low percentage of camphor (0.5 %). The use of headspace SPME was shown to be a convenient and effective analytical tool for the sampling of volatile compounds and it could be used to test the quality of flowers and essential oils from Lavandula species.     

Development of gas chromatography-mass spectrometry with microwave distillation and simultaneous solid-phase microextraction for rapid determination of volatile constituents in ginger

In this study, gas chromatography-mass spectrometry (GC-MS) following microwave distillation and solid-phase microextraction (MD-SPME) was developed for the analysis of essential oil compounds in fresh ginger. In the proposed method, the isolation, extraction and concentration of volatile components in ginger were carried out in one single step, using the MD-SPME technique, and the analytes on the SPME fiber were analyzed by GC-MS. Some parameters, including SPME fiber coating, microwave power and irradiation time, were optimized. The optimal experiment parameters obtained were: 65 microm PDMS/DVB SPME fiber, a microwave power of 400 W and an irradiation time of 2 min. To demonstrate its feasibility, MD-SPME was compared with conventional SPME for the extraction of essential oil compounds in fresh ginger. Using MD-SPME followed by GC-MS, 54 compounds were separated and identified in ginger, which mainly included geranial (5.25%), zingiberene (15.48%), beta-sesquiphellandrene (5.54%) and beta-phellandrene (22.84%), whereas only 39 compounds were separated and identified by conventional SPME followed by GC-MS. The relative standard deviation (R.S.D.) values of less than 10% show that the proposed method has good repeatability. The result show that MD-SPME, followed by GC-MS, is a simple, rapid, solvent-free method for the determination of volatile compounds in ginger.     

激光拉曼光谱快速测定中药姜黄

目的 应用激光拉曼光谱无损快速测定姜黄.方法 采集姜黄的拉曼光谱图,并结合二阶导数对其进行定性分析.结果 姜黄拉曼光谱谱中出现了1629、1596、1433、1250、1150、962、943、481 cm-1等较强的特征峰,主要归属为姜黄素类化合物和氨基酸、多糖等物质,与已知姜黄生化成分基本相符,根据谱图信息可建立姜黄的拉曼指纹图谱.应用二阶导数谱,可对结果进行进一步补充验证说明.结论 拉曼光谱技术可用于姜黄的快速测定.