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正交实验法优选肠泻停胶囊的提取工艺 被引量:2
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作者 窦芳 陈晓莉 文爱东 《陕西中医》 2012年第12期1667-1669,1680,共4页
目的:优选肠泻停胶囊的提取工艺条件。方法:以盐酸小檗碱、鞣质含量为指标,采用L9(34)正交实验,优选肠泻停胶囊的最佳提取工艺。结果:黄柏加7倍量的70%乙醇热回流提取3次,每次1.5h。醇提后的黄柏药渣、地榆、石榴皮和地锦草,用15倍量的... 目的:优选肠泻停胶囊的提取工艺条件。方法:以盐酸小檗碱、鞣质含量为指标,采用L9(34)正交实验,优选肠泻停胶囊的最佳提取工艺。结果:黄柏加7倍量的70%乙醇热回流提取3次,每次1.5h。醇提后的黄柏药渣、地榆、石榴皮和地锦草,用15倍量的水煎3次,每次1.5h。结论:利用最佳的工艺条件能充分有效的提取肠泻停胶囊方中药材的有效成分。 展开更多
关键词 @肠泻停胶囊 工艺小檗碱 分析高效相色谱法
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Analysis of the monosaccharide composition of fucoidan by precolumn derivation HPLC 被引量:6
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作者 张晶晶 张全斌 +2 位作者 王晶 石学连 张忠山 《Chinese Journal of Oceanology and Limnology》 SCIE CAS CSCD 2009年第3期578-582,共5页
We developed an HPLC method for analysis of the monosaccharide composition of fucoidans. The fucoidan was hydrolyzed into monosaccharides with 2 mol/L trifluoroacetic acid. Using ribose as the internal standard, the m... We developed an HPLC method for analysis of the monosaccharide composition of fucoidans. The fucoidan was hydrolyzed into monosaccharides with 2 mol/L trifluoroacetic acid. Using ribose as the internal standard, the monosaecharide derivatives, obtained with 1-Phenyl-3-methyl-5- pyrazolone (PMP), were separated by reverse-phase HPLC using a gradient elution process, and monitored by ultraviolet detection at 245 nm. In the concentration range of 0.1-2.0 mmol/L, the peak area of each monosaccharide had a good linear relationship with its concentration (r^2〉0.998). The average recoveries of mannose, rhamnose, glucuronic acid, glucose, galactose, xylose, and fucose were 86.2%, 95.1%, 62.5%, 102.0%, 94.8%, 66.6%, and 105.1%, respectively. This method was accurate and had good reproducibility and could be used to determine the monosaccharide contents of fucoidans. 展开更多
关键词 FUCOIDAN MONOSACCHARIDE DERIVATION HPLC
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Microanalysis and preliminary pharmacokinetic studies of a sulfated polysaccharide from Laminariajaponica 被引量:4
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作者 张文静 孙德林 +3 位作者 赵峡 金维华 王晶 张全斌 《Chinese Journal of Oceanology and Limnology》 SCIE CAS CSCD 2016年第1期177-185,共9页
A rapid, sensitive and reproducible high performance liquid chromatography (HPLC) method with post-column fluorescence derivatization has been developed to determine the amount of low-molecular- weight sulfated poly... A rapid, sensitive and reproducible high performance liquid chromatography (HPLC) method with post-column fluorescence derivatization has been developed to determine the amount of low-molecular- weight sulfated polysaccharide (GFS) in vivo. The metabolism of GFS has been shown to fit a two component model following its administration by intravenous injection, and its pharmacokinetic parameters were determined to be as follows: half-time of distribution phase (t1/2α)=11.2±2.93 min, half-time of elimination phase (tl/2α)=98.20±25.78 min, maximum concentration (Cmax)=110.53 gg/mL and peak time (Tmax)=5 min. The pharmacokinetic behavior of GFS was also investigated following intragastric administration. However, the concentration of GFS found in serum was too low for detection, and GFS could only be detected for up to 2 h after intragastric administration (200 mg/kg body weight). Thus, the bioavailability of GFS was low following intragastric administration because of the metabolism of GFS. In conclusion, HPLC with post-column derivatization could be used for quantitative microanalysis and pharmacokinetic studies to determine the presence of polysaccharides in the serum following intravenous injection. 展开更多
关键词 sulfated polysaccharide HPLC post-column derivatization MICROANALYSIS PHARMACOKINETICS
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Component Analysis of Volatile Oil of Garlic from Different Districts and Assay of Allicin Content 被引量:2
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作者 WANG Ying WU Wen-li +2 位作者 WANG Bin WANG Dao-ping HAO Xiao-yan 《Chinese Food Science》 2012年第1期40-42,50,共4页
[ Objective] The aim was to study the chemical component of volatile oil of garlic in different districts. [ Method] GC-MS was used to an- alyze the composition of the garlic volatile oil in Guiyang, Guizhou Majiang, ... [ Objective] The aim was to study the chemical component of volatile oil of garlic in different districts. [ Method] GC-MS was used to an- alyze the composition of the garlic volatile oil in Guiyang, Guizhou Majiang, Shandong, Yunnan and Chongqing and the HPLC method was used to assay the content of gadicin. [ Result]Gadicin in different essential oil had the highest content but varied a lot. The sampling amount of garlicin be- tween 0.562 and 2.810 μg was in a good linear relation (R =0.999 2, n = 5 ) with peak area, the average recovery rate was 99.39, RSD = 1.76%. [ Conclusion] GC-MS can be used to analysis the composition of essential oil quickly and effectively. The liquid chromatographic analysis of garlicin was simple, reliable and reproducible. The study provided the theoretical basis for selecting garlic in gadic flavor oil production and improving quality of gadicin oil. 展开更多
关键词 GARLIC ALLICIN Volatile oil GC-MS HPLC Content assaying China
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Economic and Qualitative Traits of Italian Alps Saffron 被引量:1
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作者 Alessandra MANZO Sara PANSERI +1 位作者 Danilo BERTONI Annamaria GIORGI 《Journal of Mountain Science》 SCIE CSCD 2015年第6期1542-1550,共9页
Saffron, obtained from the flower stigmas of Crocus sativus L., is one of the most expensive food spices. The introduction of saffron in alpine areas could help to broaden and diversify the activities of mountain mult... Saffron, obtained from the flower stigmas of Crocus sativus L., is one of the most expensive food spices. The introduction of saffron in alpine areas could help to broaden and diversify the activities of mountain multifunctional farms, with a positive impact on economy and land management. According to ISO 3632(2010/2011), saffron can be classified into three categories of quality(I, II, III) depending on the concentration of the three main metabolites responsible for its characteristic colour, flavor and aroma: Crocin, Picrocrocin and Safranal. This study represents the first investigation of the quality of saffron produced in the Italian Alps evaluated with spectrophotometry, HPLC, solid-phase microextraction(SPME), and gas chromatographic analysis combined with mass spectrometry(GC/MS). The experiments used Crocus sativus stigmas produced in 2012-2013 in different areas of the Central Italian Alps were located at an altitude between 720 and 1200 m a.s.l.. Results obtained were compared to commercial saffron. The analyses confirmed that all samples can be classified in the first quality category according to the ISO classification. This high quality is also confirmed by HPLC analysis. Moreover, the SPME-GC/MS analysis identified some differences in the aromatic profile of saffron samples, in particular regarding safranal concentration. A preliminary assessment of the economic viability of high quality saffron production for local markets was also performed. Our study provides valid information regarding the quality and economic sustainability of saffron production in the alpine area confirming this crop as a good candidate for a new source of income for multifunctional farms in mountain areas. 展开更多
关键词 Crocus sativus L. Alps ISO 3632 UV– Vis spectrophotometry SPME-GC/MS HPLC
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Ultrafiltration of Shiitake Polyphenol with Ultrasound Enhancement
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作者 Defang SHI Hong GAO +3 位作者 Xiuzhi FAN De YANG Shujing XUE Wei CHENG 《Agricultural Science & Technology》 CAS 2015年第10期2243-2246,共4页
Ultrafiltration (UF) experiments were subjected to the concentration of Shi- itake polyphenol(SP) with ultrasound (US) enhancement, by which the effects of the main parameters such as ultrasonic power, transmemb... Ultrafiltration (UF) experiments were subjected to the concentration of Shi- itake polyphenol(SP) with ultrasound (US) enhancement, by which the effects of the main parameters such as ultrasonic power, transmembrane pressure, temperature and axial flow-rate on the membrane fluxes were analyzed, and then the SP of the ultrafiltrate after follow-up resin adsorption by HPLC was investigated. The results in- dicated that US could significantly enhance the membrane fluxes. The optimal con- ditions obtained was as follows: 0.60 W/cm2 US power, axial flow-rate of 80 L/h, operation temperature 30 ~C, transmembrane pressure 0.10 MPa. US increased the absorption capacity of the absorbent resin during the following stage. The HPLC analysis also showed that catechins were purified to some extent as the ultrafiltrate was treated by US and macroporous resin, indicating the technology of US en- hancement coupled with UF showed the potential for concentration and purification of SP by absorbent resins. 展开更多
关键词 SHIITAKE ULTRAFILTRATION ULTRASOUND
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Optimization of Yield and Chemical Properties of Agar Extracted from Melanothamnus Somalensis from Oman Sea
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作者 Zainab Mohammed Al-Nahdi Ahmed Al-Alawi +1 位作者 Insaaf Al-Marhobi Ali Al-Zefiti 《Journal of Environmental Science and Engineering(B)》 2015年第6期302-314,共13页
The red seaweed Melanothamnus somalensis was investigated as potential economic source of agar. The effect of different conditions of alkali pre-treatment on chemical properties of agar was evaluated. Agar was extract... The red seaweed Melanothamnus somalensis was investigated as potential economic source of agar. The effect of different conditions of alkali pre-treatment on chemical properties of agar was evaluated. Agar was extracted by various concentrations of NaOH (4%, 6% and 8%) and heated at different temperatures (70 ℃, 75 ℃ and 80 ℃) for different durations (2 h, 2.75 h and 3.5 h). The yields-molecular weight (Mw) and sulfate contents of extracted agar were analysed and characterized by FTIR spectroscopy. The yield was significantly increased at these treatments from 23.29% to 30.86%. Mw studied by HPLC ranged from (.12.45 ± 0.21) × 10^5 to (8.60 ± 2.40) × 10^5 Da. FTIR bands show sulfate groups in C4 and C6 ofgalactose and no sulfate group were found on both C2 of galactose and C2 of 3,6-anhydrogalactose. All treatments showed a high sulfate content that ranged from 5.4% to 10.1%. These properties were found to be significantly affected by the alkali pre-treatment concentration (p 〈 0.05). In conclusion, agar extracted in this study was considered acceptable for industrial application and the optimal conditions for extraction were found to be at 6% NaOH at 70 ℃ for 2 hours. 展开更多
关键词 SEAWEED Melanothamnus somalensis agarophytes agar extraction alkali pre-treatment FTIR.
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Development of a chiral HPLC method for the analysis of naftopidil enantiomers 被引量:1
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作者 孙银香 黄碧云 +1 位作者 袁牧 石京山 《Journal of Chinese Pharmaceutical Sciences》 CAS 2009年第1期61-63,共3页
We developed a chiral HPLC method for the separation and analysis ofnaftopidil enantiomers. The two enantiomers of naflopidil were separated using a Chiralpak AD-H (250 mm×4.6 mm, 5 μm) column and monitored at... We developed a chiral HPLC method for the separation and analysis ofnaftopidil enantiomers. The two enantiomers of naflopidil were separated using a Chiralpak AD-H (250 mm×4.6 mm, 5 μm) column and monitored at the wavelength of 283 nm. The isocratic mobile phase consisting of hexane-isopropanol-diethylamine (85:15:0.1, v/v/v) was pumped at a flow rate of 1.0 mL/min. Under these chromatographic conditions, R-naflopidil and S-naftopidil were well separated and had good linearity in the ranges of 0.78-50 μg/mL (r = 0.9999) and 0.84-54 μg/mL (r = 0.9998), respectively. The relative standard deviations (RSD) of intra- and inter-day assays were no more than 0.5% and 0.7%, respectively. This improved method for the separation and quantitative determination of naflopidil enantiomers can be used for the quality control of synthesized naflopidil product. 展开更多
关键词 ENANTIOMERS NAFTOPIDIL Chiral HPLC ANALYSIS
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