气相色谱-质谱联用结合化学计量学分辨法分析甘松的挥发油成分

目的分析中药甘松的挥发油成分。方法采用气相色谱-质谱联用(GC-MS)结合化学计量学分辨法对甘松挥发油成分进行定性分析,对重叠峰和包埋峰采用直观推导式演进特征投影法(HELP)和选择离子法(SIA)进行分辨,同时计算各组分的程序保留指数(PTRI),用NIST质谱库对解析后的纯组分进行定性。结果定性分析出69种化学成分,占总含量的93.98%。结论 GC-MS法结合化学计量学分辨法比单用GC-MS法定性结果更加准确、可靠。     

气相色谱-质谱和化学计量学解析法分析药对麻黄-桂枝挥发油成分

利用气相色谱-质谱对药对麻黄-桂枝及单味药麻黄和桂枝的挥发油成分进行检测，通过化学计量学解析法对产生的二维色谱-质谱数据进行解析，得到各组分的纯色谱和质谱，根据其保留时间和质谱，在质谱库中进行相似检索，实现对组分的定性，再用总体积积分法进行定量。麻黄-桂枝、麻黄和桂枝挥发油分别定性了97，72和68个色谱峰，占总含量的89.76%，90.08%和91.62%。药对挥发油成分的数目大致为麻黄和桂枝挥发油成分的加和，但相对含量有变化。     

气相色谱-质谱分析蒲公英挥发油成分

采用气相色谱-质谱联用技术对蒲公英挥发油成分进行分析。结果分离出19个成分，鉴定了其中的15个成分，主要为2-呋喃甲醛：测定了其中各成分的含量。     

气相色谱-质谱技术分析中药丁香挥发油成分

目的:应用气相色谱-质谱(GC-MS)分析出中药丁香挥发油中的化学成分。方法:利用水蒸气蒸馏的方法提取中药丁香挥发油,并结合GC-MS技术对其成分进行检测。结果:中药丁香挥发油中共检测出4种成分,其中主要成分是3-烯丙基-2-甲氧基苯酚,占总成分的69.77%。结论:中药丁香挥发油的主要成分是3-烯丙基-2-甲氧基苯酚。     

气相色谱-质谱和化学计量学解析法分析防风挥发油成分

目的：定性、定量分析防风挥发油成分。方法：采用气相色谱-质谱法进行检测，通过化学计量学解析法对重叠色谱峰进行分辨，实现防风挥发油成分的定性、定量分析。结果：防风挥发油成分鉴定了45个，占挥发油成分总含量的89．15％。结论：防风挥发油主要成分是镰叶芹醇（11．24％），苯亚甲基苯甲醛（9．40％），正辛醛（6．76％），正己醛（3．16％），2，3，5，6，7，8，8a-八氢-1，4-二甲基-7-（1-甲基乙烯基）莫（2．13％），2，4-癸二烯醛（1．83％）和正庚醛（1．71％）．     

砂仁挥发油成分的气相色谱-质谱分析

目的分析砂仁的挥发油成分,鉴定砂仁质量。方法以水蒸气蒸馏法提取砂仁挥发油,分别得到不同样品的挥发油,采用气相色谱-质谱(GC-MS)技术对其化学成分进行分离鉴定,并与标准图谱对照,确定化合物成分,经色谱峰面积归一法测定其百分含量。结果市售砂仁中乙酸龙脑酯的含量为25.14%(越南砂仁)～69.32%(广东春砂仁)。结论乙酸龙脑酯含量最高为广东春砂仁,进一步证实砂仁以广东春砂仁为道地品种。     

川木香挥发性成分的气相色谱-质谱分析

目的:时川木香挥发性成分进行气相色谱-质谱分析.方法:采用水蒸气蒸馏法从川木香中提取挥发油,用气相色谱-质谱法对木香挥发油进行化学成分的分析.并用色谱峰总体积积分和归一化法获得各化合物的相对含量.结果及结论:共鉴定了52种化合物,占挥发油总成分的92%以上.其中主要有Cycloisolongifolene,8,9-dehydro-9-formyl-,Mokko lactone,Dehydrocostuslactone等.     

月见草全草挥发油成分的气相色谱-质谱联用分析

目的:分析柳叶菜科月见草属植物月见草挥发油的化学成分。方法:用水蒸气蒸馏法提取月见草全草挥发油,并用气相色谱-质谱联用(GC-MS)法对挥发油成分进行分析。结果:共分离了30个峰,确认了其中22个化合物,其中含量最多的是去氢香薷酮(89.02%)。结论:首次采用气相色谱-质谱联用法分析月见草全草挥发油的化学成分,为月见草的进一步研究及开发利用提供了科学依据。     

GC-MS和化学计量学解析法分析白术中挥发油成分

目的 分析白术挥发油中的化学成分。方法 采用气相色谱-质谱(GC-MS)联用技术对其进行分离检测,利用化学计量学解析法(CRM)对重叠色谱峰进行分辨解析,并结合程序升温保留指数辅助定性,从而对挥发油成分进行准确的定性定量分析。结果 共分辨出了33个色谱峰,鉴定了其中29个组分,占白术挥发油总量的95.93%,其中主要化学成分为2-(2-甲氧基)苯甲氧基苯酚、γ-芹子烯和3,7(11)-蛇床二烯等,它们占总挥发油的70.07%,而其他26个组分只占25.86%。结论 结合使用CRM解析重叠色谱峰,比单独使用GC-MS能更真实、全面地反映白术中的挥发油化学成分。     

GC-MS和化学计量学解析法分析白术中挥发油成分

目的分析白术挥发油中的化学成分。方法采用气相色谱-质谱（GC-MS）联用技术对其进行分离检测,利用化学计量学解析法（CRM）对重叠色谱峰进行分辨解析,并结合程序升温保留指数辅助定性,从而对挥发油成分进行准确的定性定量分析。结果共分辨出了33个色谱峰,鉴定了其中29个组分,占白术挥发油总量的95.93%,其中主要化学成分为2-（2-甲氧基）苯甲氧基苯酚、γ-芹子烯和3,7（11）-蛇床二烯等,它们占总挥发油的70.07%,而其他26个组分只占25.86%。结论结合使用CRM解析重叠色谱峰,比单独使用GC-MS能更真实、全面地反映白术中的挥发油化学成分。     

Analysis of volatile oil in Rhizoma ligustici chuanxiong-Radix paeoniae rubra by gas chromatography-mass spectrometry and chemometric resolution

AIM: To analyze the volatile chemical components of the herbal pair Rhizoma Ligustici chuanxiong-Radix paeoniae rubra (RLC-RPR) and compare them with those of each of the herbs alone. METHODS: Gas chromatography-mass spectrometry (GC-MS), a chemometric resolution technique using the heuristic evolving latent projections (HELP) method, and the overall volume integration method were used. RESULTS: In total, 52, 38, and 61 volatile chemical components in RLC, RPR, and RLC-RPR essential oils were determined, respectively, accounting for 95.14%, 95.19%, and 89.68% of the total contents of essential oil of RLC, RPR, and RLC-RPR, respectively. The main volatile chemical components were butyldienephthalide (20.65%) and ligustilide (50.15%) for RLC; and n-hexadecanoic acid (20.18%), [Z,Z]9,12-octadecadienoic acid (30.11%), 2-hydroxy-benzaldehyde (17.08%) for RPR, and butyldienephthalide (14.80%), and ligustilide (38.91%) for RLC-RPR. The main volatile chemical components of RLC-RPR were almost the same as those of RLC, but the relative amounts were altered. CONCLUSION: The number of volatile chemical components in RLC-RPR was almost equal to the sum of the number in the 2 constituent herbs, but the relative amounts were altered. Furthermore, an acid-base reaction takes place during the process of decocting the herbs. The data gathered in this study may be helpful for understanding the synergistic nature of this herb pair in traditional Chinese medicine.     

GC-MS法检测中草药保健食品中的农药多残留

目的建立一种检测保健食品中的农药多残留的分析方法。方法样品用乙腈提取并经硅胶柱净化后供GC-MS分析。采用选择离子扫描方式,内标标准曲线法定量。结果 20种农药在47 min内达到理想的分离效果。以3个添加水平测定样品的回收率和相对标准偏差,回收率在72.95%和118.48%之间,RSD均小于13%。各农药检测限为0.001 0～0.004 4 mg·kg-1。结论该方法简便、快速、准确、灵敏,且重现性好,可用于中草药保健食品中多种农药残留的同时测定。     

Analysis of adulterants in a traditional herbal medicinal product using liquid chromatography-mass spectrometry-mass spectrometry

Adulterations with synthetic drugs are common problems with herbal medicine and this can potentially cause serious adverse effects. It is therefore important to determine the presence of synthetic drugs in herbal medicine to ensure patients' safety. The objective of this study was to develop sensitive and specific methods to analyse phenylbutazone, caffeine and oxyphenbutazone present in a traditional Indonesian herbal product. Liquid chromatography-mass spectrometry-mass spectrometry (LC-MS-MS) methods in the selected reaction-monitoring (SRM) mode were developed. It was found that the sample contained 0.53% w/w (n=3, RSD=7.56%) phenylbutazone and 0.04% w/w (n=3, RSD=8.39%) caffeine. This corresponded to 43.17 mg phenylbutazone and 3.23 mg caffeine in each sachet of powder. The methods were validated for linearity, precision, accuracy, LOD and LOQ. LOD and LOQ were found to be 3.69 and 12.29 ng/ml, respectively for phenylbutazone. For caffeine, the LOD and LOQ were 0.84 and 2.80 ng/ml, respectively. Oxyphenbutazone in the sample was found to be present at a level below the quantification level of 10.2 ng/ml. With better methods developed for analysis of adulterants in herbal medicine, the quality and safety of these medicines can be better controlled and regulated to ensure patients' safety.     

Analyzing of the volatile chemical constituents in Artemisia capillaris herba by GC-MS and correlative chemometric resolution methods

The volatile chemical constituents in traditional Chinese medicine (TCM), Artemisia capillaris herba, were determined by gas chromatography-mass spectrometry (GC-MS). The acquired two-dimensional data were resolved by correlative chemometric resolution methods. The noise in the raw data is pretreated by roughness penalty smoothing method. With the data denoised, heteroscedastic noise and signal-to-noise ratio were decreased apparently, which was favorable to the determination of component number. The selective range can be extracted from rankmap obtained by fixed size moving window evolving factor analysis (FSMWEFA) conveniently. The overlapped chromatographic peaks were resolved into pure chromatograms and pure spectra with evolving window orthogonal projection (EWOP). The purity of the resolved pure spectra were improved furthermore with the heteroscedastic noise decreased through roughness penalty smoothing method, although the basic structure of the raw data changes little. Qualitative analysis was performed by similarity search in NIST147 and Willey library. Pure chromatograms are in favor of quantitative analysis, which was obtained by total volume integration. Forty-two of seventy-five separated constituents in essential oil, accounting for 89.03% of the total content, were identified. The result proves the combined approaches to be powerful for the analysis of complex herbal samples.     

气相色谱/质谱和化学计量学解析法用于千斤拔挥发性成分的分析

目的:研究蔓性千斤拔的挥发性成分。方法:利用水蒸气蒸馏法提取蔓性千斤拔挥发油,用GC-MS检测,用子窗口因子分析法(SFA)分辨重叠色谱峰,从而获得每一组分的纯色谱和质谱,依靠每一组分纯质谱在NIST质谱库进行相似性检索而定性分析,用总体积积分法进行定量分析。结果:共分辨出76个色谱峰,鉴定出59个化学成分,占总含量的86.58%。主要组分为金合欢醇、β-愈创烯、α-雪松烯、长叶环烯、γ-雪松烯和β-雪松烯。结论:本文提出的方法不仅可鉴定的化合物数目增加,而且也提高了定性准确度,该法能用于千斤拔的进一步开发和质量控制。     

Screening and analysis of bioactive compounds in traditional Chinese medicines using cell extract and gas chromatography-mass spectrometry

As the cost of drug development is always many times more than that of drug discovery, predictive methods aiding in the screening of bioavailable drug candidates are of profound significance. In this paper, a novel method for screening bioactive compounds from traditional Chinese medicines (TCMs) was developed by using living cell extract and gas chromatography (GC)-mass spectrometer (MS). The method was validated by using elemene emulsion injection (EEI), a typical TCM with known active compound, to interact with murine ascites hepatocarcinoma cell strain with high metastatic potential (HCa-F). Finally, the method was applied to screen the bioactive compounds from multi-component zedoary turmeric oil and glucose injection (ZTOGI). After HCa-F cells was incubated in ZTOGI, ethyl acetate (EtOAc) was used to extract the compounds in the cells for GC-MS analysis. Fourteen compounds were detected in the desorption eluate of HCa-F cell extract of ZTOGI, and further identified by MS. Curzerene and beta-elemene were found to be two major bioactive compounds in ZTOGI. These results show that the method developed may be applied to quickly screen the potential bioactive components in TCMs interacting with the target cells.     

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.