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冠心苏合丸中挥发性成分的提取分析及其质量监控 总被引:1,自引:0,他引:1
采用了水蒸气蒸馏 萃取法和同时水蒸气蒸馏 萃取法提取冠心苏合丸中的挥发性组分,测得用两种方法提取的冠心苏合丸中的挥发性组分提取率分别为11%和14%。利用GC MS方法对两种方法所得的挥发性组分进行分析,通过G1701BA化学工作站检索NIST98谱图库,并结合标准谱图库和有关文献,从冠心苏合丸中的挥发性组分中分别确定出19种、14种化学成分,分别占冠心苏合丸中挥发性组分总检出量的95.89%和97.27%。用峰面积归一化法通过化学工作站数据处理系统,得出各化学成分在挥发性组分中的质量分数。主要挥发性组分是冰片、异冰片和苯甲酸苄酯。从两种方法提取的挥发性组分中确认的化学成分是否涵盖五味中药材具有代表性成分,可以很方便地进行质量监控和真伪鉴别。并采用气相色谱法对冠心苏合丸中冰片的含量进行了测定,作为辅助鉴别。结果,冰片浓度在1.0~5.0mg mL范围内与冰片对内标物的色谱峰面积比值成良好的线性关系,冰片的平均回收率为98%~106%。 相似文献
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千山野菊花挥发性化学成分的提取与分析 总被引:3,自引:0,他引:3
报道了用蒸馏-萃取法和同时蒸馏-萃取法提取千山野菊花中挥发性物质,测得用两种方法提取的千山野菊花挥发油含量分别为6.1%和7.0%,用GC/MS法从千山野菊花挥发油中分别分离并确定出34种和29种化学成分,分别占千山野菊花挥发油总检出量的89.47%和90.72%,用峰面积归一化法得出各类化学成分在挥发油中的相对百分含量。 相似文献
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本文应用气相色谱-傅里叶变换红外光谱联用技术对中成药冠心苏合丸中挥发性成分进行了库检索,鉴定了其中7种有效成分,并采内标法对其中龙脑、异龙脑的总量进行了含量测定,其平均回收率为98.53%。 相似文献
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姜科姜黄属植物有效成分的研究 总被引:13,自引:0,他引:13
研究不同产地姜科姜黄属植物挥发油的化学成分,了解不同产地姜科姜黄属植物挥发性成分的差别,为控制其药材质量提供理论依据。采用水蒸气蒸馏法提取不同产地姜科姜黄属植物的挥发油,用气相色谱—质谱联用仪对其进行分离测定,结合计算机检索对分离的化合物进行结构鉴定,应用色谱峰面积归一化法测定各成分的相对百分含量。结果发现,不同产地姜科姜黄属植物的水蒸气蒸馏提取物得率在0.20%~2.13%之间,分别鉴定出24~40个化学成分。不同品种、不同产地姜科姜黄属植物的挥发油含量和其所含成分有较大差别,文献报道的某些有效成分如莪术酮、莪术二酮、莪术醇和表莪术酮在某些供试品中未检测到。实验中10个供试品药材中挥发性成分主要为单萜类及倍半萜类化合物及其衍生物,倍半萜类化合物的百分含量(44.57%~88.65%)明显高于单萜类化合物的百分含量(1.63%~26.69%)。 相似文献
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复方祛风湿止痛药粉末中挥发性成分的静态顶空-气相色谱-质谱分析 总被引:3,自引:0,他引:3
利用静态顶空-毛细管气相色谱-质谱方法对复方祛风湿止痛药中挥发性成分进行了分析,运用质谱检索和保留指数对其中主要的60种挥发性成分进行了定性.该药中各种挥发性成分的相对含量分别为萜类(54.5%)、萜类衍生物(9.6%)、酚醚类(15.0%)和脂肪醇醛(8.5%),主要为β-古芸烯(20.5%)、蒿脑(14.5%)、β-蛇床烯(6.0%)和β-绿叶烯(5.7%).分析结果的相对标准偏差(RSD)在0.54%~8.39%之间. 相似文献
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自动化静态顶空-气相色谱-质谱对天然香精中挥发性化学成分的快速分析 总被引:13,自引:3,他引:13
运用静态顶空-毛细管气相色谱-质谱法对天然香精中挥发性化学成分进行了分析,采用质谱和保留指数检索结合的方法对香精中挥发性成分进行定性分析;对香精顶空分析条件进行了优化,在香精样品中加入适量饱和NaCI溶液,显著地提高了低极性挥发性组分的分析灵敏度;从该香精中检出了68个化合物,将峰面积归一化结果大于0.1%的60种挥发性成分进行了定性分析,并通过保留指数分析对其中45种化合物进行了确认;分析结果表明:香精中含有萜类(30.3%)、萜类衍生物(11.7%)、酚醚类(17.0%)、脂肪酸酯(20.9%)和一些小分子的缩醛类化合物(17.7%),其中主要的挥发性成分为丁酸-1,1-二甲基-苯基乙酯(18.9%)、茴香脑(15.6%)、2-乙基-4-甲基-1,3-二氧戊环(9.8%)和β-石竹烯(7.7%);对方法精密度进行考察.相对标准偏差(RSD)在0.62—9.36之间。 相似文献
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The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted
indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator
model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was
established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing
analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997. 相似文献
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Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared. 相似文献
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Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position. 相似文献
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Stepkowska E. T. Perez-Rodriguez J. L. Jimenez de Haro M. C. Sayagues M. J. 《Journal of Thermal Analysis and Calorimetry》2002,69(1):187-204
Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, Mo, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献
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The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations
were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples
were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of
hematite Fe2O3. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the
best fitting experimental data.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
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Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6. 相似文献
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