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1.
??OBJECTIVE To develop a method of quantitative analysis of multicomponents by singlemarker (QAMS) for simultaneous determination of six oligosaccharide esters in Polygalae Radix. METHODS 3,6??-Disinapoyl sucrose (DISS) was used as the internal reference substance. The relative correlation factors (RCF) of sibiricose A5, sibiricose A6, tenuifoliside B, tenuifoliside A, and tenuifoliside C to DISS were calculated. The contents of the six oligosaccharide esters in 20 different batches of Polygalae Radix were determined by both external standard method and QAMS. The assay results were compared to evaluate the accuracy of QAMS method. RESULTS The RCF of sibiricose A5, sibiricose A6, tenuifoiside B, tenuifoliside A, and tenuifoiside C to DISS were 1.23, 1.16, 1.56, 1.79, and 0.92, respectively. Under different experimental conditions, the RCF had good reproducibility, and there was no significant difference in the quantitative analysis results between the external standard method and QAMS method. CONCLUSION The QAMS method is feasible and credible, and can be used for the quality control of oligosaccharide esters in Polygalae Radix.
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2.
??OBJECTIVE To establish a method for content determination of ginsenoside Rg1, ginsenoside Rb1, saikosaponin a, saikosaponin d, and saikosaponin B2 in 70% ethanol elution effective fraction of Chaihu plus Longgu Muli decoction by HPLC-ELSD. METHODS A Diamonsil C18 column(4.6 mm??250 mm, 5 ??m) was used as the stationary phase and the mobile phase consisted of acetonitrile and water. Gradient elution was carried out at the flow rate of 1.0 mL??min-1. The column temperature was maitained at 30 ??. The ELSD detector was operated at 105 ?? with nebulizing gas at the optimum flow rate of 2.5 L??min-1. RESULTS The average contents of ginsenoside Rg1, ginsenoside Rb1, saikosaponin a, saikosaponin d, and saikosaponin B2 were 0.474%, 1.372%, 1.554%, 0.883%, and 2.073%, respectively. The calibration curves were linear in the ranges of 1.820-9.10, 1.810-9.050, 1.130-10.170, 0.420-2.100, and 3.125-15.625 ??g, respectively. The RSDs of precision, reproducibility and recovery were all less than 3.0%. CONCLUSION The method is rapid, simple, reliable and accurate, and has been successfully used to the quantification of five components in 70% ethanol elution effective fraction of Chaihu plus Longgu Muli decoction, which can provide a basis for the quality evaluation of Chaihu plus Longgu Muli decoction. 相似文献
3.
??OBJECTIVE To develop a method of quantitative analysis of multi-components by single marker(QAMS) for simultaneous determination of five compounds in extract of Penthorum chinense Pursh. METHODS A HPLC method was established on an Agilent ZORBAX SB-C18 column(4.6 mm??250 mm, 5 ??m). The mobile phase was acetonitrile-0.2% formic acid aqueous solution. Gradient elution was performed at a flow rate of 1.0 mL??min-1. The column temperature was 30 ?? and the detection wavelength was set at 280 nm. Pinocembrin-7-O-??-D-glucoside was selected as the internal reference substance, and the relative correlation factors(RCF) of gallic acid, brevifolin carboxylic acid, 2, 6-dihydroxyacetophenone-4-O-??-D-glucoside, quercetin-3-O-??-D-xyloside and quercetin-3'-O-??-L-rhamnoside were determined by HPLC. The contents of the six components were determined by both QAMS method and external standard method and the RESULTS were compared. The accuracy and feasibility of the new method were validated by QAMS method and external standard method. RESULTS No significant differences were observed in the determination RESULTS of five constituents except brevifolin carboxylicacid in 21 batches of extract of P. chinense by QAMS method and external standard method. CONCLUSION The QAMS method is feasible and suitable to determine the contents of five constituents in the extract of P. chinense. 相似文献
4.
??OBJECTIVE To develop a simultaneous quantitative analysis method of four triterpenoids in Alismatis Rhizoma by multi-components by single maker (QAMS). METHODS Four main triterpenoids (alisol A, alisol A 24-acetate, alisol B and alisol B 23-acetate) were selected as analytes to evaluate the quality of Alismatis Rhizoma. Alisol B 23-acetate was used as the internal reference standard and three relative correction factors (RCFs) to alisol B 23-acetate were calculated. These RCFs were obtained by high performance liquid chromatography coupled with diode array detector under various chromatographic conditions. Then 31 batches of Alismatis Rhizoma samples collected from different areas were determined by both external standard method (ESM) and QAMS. RESULTS The RCFs were obtained with good reproducibility (RSD ?? 2.25%). No obvious differences were observed between the analysis results of QAMS method and ESM method (RSD ?? 3.52%). CONCLUSION The established QAMS method is reliable and feasible for simultaneous analysis of four triterpenoids and could be used for quality control of Alismatis Rhizoma. 相似文献
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??OBJECTIVE To establish HPLC methods for the determination of betulinic acid, oleanolic acid, ursolic acid, and lupeol in Caragana sinica roots, and investigate the ??-glucosidase activity of the four compounds in vitro. METHODS An Agilent Eclipse XDB-C18 column (4.6 mm??250 mm, 5 ??m) was applied with methanol-water-phosphoric acid (85:15:0.1) as the mobile phase at a flow rate of 0.6 mL??min-1 to separate betulinic acid, ursolic acid, and oleanolic acid. An Inert Sustain C18 column (4.6 mm??150 mm,5 ??m) was applied with acetonitrile-water (70:30) as the mobile phase at a flow rate of 0.8 mL??min-1 to separate lupeol. RESULTS Good linearities were achieved for betulinic acid, oleanolic acid, ursolic acid, and lupeol within the range of 0.56-5.58, 0.42-4.20, 0.19-1.92, and 6.10-61.00 ??g, respectively. The average recoveries were 99.79%, 98.51%, 98.05%, and 99.47%, and the RSDs were 1.53%,1.74%,1.78%, and 1.94%, respectively. CONCLUSION The developed methods are accurate and can be used for the quality control of Caragana sinica. In addition to betulinic acid, the other three compounds show good ??-glucosidase inhibitory activity and are expected to be developed as new hypoglycemic drugs. 相似文献
6.
??OBJECTIVE To investigate the effect of solvent pH on the physical/chemical properties and clinical use of four drugs commonly used in gynecology and obstetrics, including aminophylline, ambroxol, labetalol and ritodrine, through simulation and evidence-based evaluation to provide theoretical guidance and quantitative reference for clinical use. METHODS By searching PubMed compound and Martindale:The Complete Drug Reference, the physical/chemical and clinical information of the four drugs were obtained. The logP, pKa, logD, and solubility were simulated using ACD/LAB 6.0 software. RESULTS The solvent pH had effects on the logD and solubility of the four drugs to a certain degree in an exponential manner. The four drugs are compatible with dextrose injection or 0.9% sodium chloride injection, but special care needs to be taken in the clinical use. CONCLUSION Solvent pH has influence on the dissolution balance of the four drugs. Simulation of the physical/chemical properties of drugs will provide theoretical guidance and reference for clinicians with more detailed information. 相似文献
7.
??OBJECTIVE To conduct the contrastive studies of universal compression model to pharmaceutical powder compression characteristics effect base on Heckel and Kawakita equation founded.METHODS The uniaxial compression tests were developed with three excipients of lactose, starch, microcrystalline cellulose and four mixture excipients of lactose, starch, microcrystalline cellulose with different mass fraction. The change rules between density and pressure and model error are analyzed of two different compression models respectively.RESULTS The absolute density error value of Heckel and Kawakita compression model is within 4%, when the pressure is greater than 80 MPa,and the variance of Kawakita model is less than Heckel model.The absolute error value of Heckel and Kawakita compression model is within 3.73%, when the pressure is larger than 60 MPa, and the variance of Kawakita compression model less than Heckel model.CONCLUSION During applying two universal compression models to analyze pharmaceutical powder compression characteristics, two models are suitable, when the pressure is between 80 and 240 MPa. 相似文献
8.
??OBJECTIVE To study the chemical constituents of Fomes fomentarius (L.Ex.Fr.). METHODS The compounds were isolated by chromatography on silica gel column, Sephadex LH-20 column, and their structures were elucidated by spectral analysis. RESULTS Six compounds were obtained and identified as fomentarinin (1), 2-hydroxy hexacosanoic acid ethyl ester (2),syringic acid (3), syringyl alcohol (4), vanillin (5), and ergosta-7,22-diene-3,6-dione (6), respectively. CONCLUSION Compound 1 is a new compound, and compound 2-6 are isolated from the fungus for the first time.
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9.
??OBJECTIVE To systematically evaluate the economics of saxagliptin for treatment of type 2 diabetes mellitus. METHODS PubMed, Embase, Cochrane Library, NHS EED, CNKI, Wanfang and CBM were systematically searched. Literatures were screened according to pre-defined inclusion criteria. The quality of included studies were evaluated by CHEERS statement and the economic RESULTS were systematically analyzed. RESULTS Eight cost-effectiveness analyses were included, one of which was conducted in China. Patients among the studies all had blood glucose non-adeguately controlled by monotherapy. When added on to metformin, saxagliptin was cost-effective compared with sulfonylureas (glipizide and glimepiride) and thiazolidinediones (pioglitazone and rosiglitazone). When added on to metformin or sulfonylureas, saxagliptin was cost-effective compared with NPH insulin. CONCLUSION Saxagliptin represents a cost-effective option in treatment of type 2 diabetes mellitus patients with non-adequately controlled blood glucose after monotherapy. 相似文献
11.
《辽宁中医杂志》2016,(2):362-367
目的:利用一测多评法建立测定苦碟子注射液中4种有机酸类成分的高效液相色谱分析方法,实现对苦碟子注射液简单、有效的质量控制。方法:以菊苣酸为内参物,测定菊苣酸与单咖啡酰基酒石酸、绿原酸、咖啡酸的相对较正因子,进而计算苦碟子注射液中有机酸的含量,并将一测多评法的计算结果与外标法实测值用相对误差进行评价,以验证一测多评法的准确性。结果:菊苣酸与单咖啡酰基酒石酸、绿原酸、咖啡酸的相对较正因子分别为1.295,1.410,0.8421,采用一测多评法对苦碟子注射液中有机酸类成分含量计算结果与外标法无显著差异,相对误差小于5%。结论:所建立的一测多评法简便、快速、可靠,可用于苦碟子注射液中有机酸类成分含量测定,为苦碟子注射液质量控制提供参考。 相似文献
12.
“一测多评”法测定甘草中6种有效成分含量 总被引:2,自引:0,他引:2
目的: 采用“一测多评”法测定甘草中6种成分的含量。方法: 采用HPLC测定甘草中6种成分的含量,流动相乙腈(A)-0.1%磷酸水溶液(B)梯度洗脱(0~20 min,90%~68% B;20~45 min,68%~30% B;45~75 min,30%~5% B),检测波长(0 min,275 nm;32 min,250 nm;33.5 min,300 nm;34.5 min,360 nm;53 min,280 nm;55 min,270 nm;57.5 min,265 nm)。以甘草酸为内标物,测定与甘草苷、甘草素、异甘草素、甘草次酸、甘草查尔酮A的相对校正因子,计算甘草中6种成分含量,并比较“一测多评”法的计算值与外标法实测值的相似度。结果: “一测多评”法和外标法测得的甘草苷、甘草素、异甘草素、甘草查尔酮A及甘草次酸的含量相似度均为0.999 9,“一测多评”法的计算值与外标法的实测值间无显著性差异。结论: 建立的“一测多评”法适用于甘草中6种有效成分的含量测定,相对校正因子可信。 相似文献
13.
目的 建立能够同时测定黄松胶囊中4种生物碱成分含量的一测多评法。方法 采用高效液相色谱法,以盐酸小檗碱为内标物,测定黄松胶囊中盐酸表小檗碱、盐酸黄连碱、盐酸巴马汀的相对校正因子,利用该相对校正因子计算其他3种生物碱的含量。结果 在线性范围内,盐酸小檗碱相对于盐酸表小檗碱、盐酸黄连碱、盐酸巴马汀的相对校正因子分别为 1.006、1.060、1.027。在不同的实验条件下相对校正因子重现性良好,4种生物碱含量计算值与实测值无显著性差异。结论 一测多评法同时测定黄松胶囊中4种生物碱成分含量准确可行。 相似文献
14.
制何首乌中四个有效成分含量的高效液相色谱法测定 总被引:1,自引:0,他引:1
目的建立高效液相色谱(HPLC)法同时测定制何首乌中二苯乙烯苷、黄豆苷元、大黄素、大黄素甲醚的方法。方法采用高效液相色谱法;色谱柱为Diamonsil C18(5μm,250 mm×4.6 mm);柱温35℃;流速1.2 ml/min;检测波长280nm;流动相为甲醇∶0.5%醋酸溶液(42∶58)。结果被测定峰与其他组分峰完全分离。二苯乙烯苷、黄豆苷元、大黄素甲醚和大黄素的线性范围分别为0.908 4~9.084μg(R2=0.999 8),0.1236~1.236μg(R2=0.999 7),0.6048~6.048μg(R2=0.999 9),0.3648~3.648μg(R2=0.999 2);平均回收率(n=6)分别为100.2%,(RSD=1.9%),98.53%(RSD=2.0%),100.7%(RSD=2.8%)和99.95%(RSD=2.0%)。结论该方法准确、简便、重复性好,可作为制何首乌中二苯乙烯苷、黄豆苷元、大黄素、大黄素甲醚的含量测定方法,并易于推广。 相似文献
15.
目的:建立桑白皮中绿原酸、东莨菪内酯、白藜芦醇、桑色素含量测定的方法。方法:采用Eclipse SB-C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈-0.01%磷酸梯度洗脱,流速1.0 m L·min~(-1),柱温30℃,检测波长285 nm。结果:绿原酸、东莨菪内酯、白藜芦醇和桑色素分别在6.4~76.8 mg·L~(-1)(r=0.999 9),5.15~61.8 mg·L-1(r=0.999 6),1.11~13.32mg·L-1(r=0.999 6),2.76~33.12 mg·L~(-1)(r=0.999 7)线性关系良好,平均加样回收率在98.4%~99.4%(RSD≤2%),供试品溶液在12 h内稳定,且该方法重复性良好;通过对5批桑白皮药材的测定,结果发现河南(批号140401)样品中绿原酸、东莨菪内酯、桑色素含量均较高,湖北(批号D5090202)样品中白藜芦醇含量相对最高。结论:该含量测定方法精密度高,准确度高,适合桑白皮中4种成分的含量测定。 相似文献
16.
Objective To apply the high performance liquid chromatography(HPLC)method to the determination of four ingredients including paeoniflorin,berberine,evodiamine,and rutaecarpin in Wuji Pellet.Methods Using Thermo-ODS2-Hypersil column(250 mm×4.6 mm,5μm)and taking acetonitrile-0.05 mol/L monopotassium phosphate as mobile phase for elution,the conditions were as follows,flow rate of 1.0 mL/min,UV detector wavelength of 225 nm,and column temperature of 25℃.Results The standard curves of paeoniflorin,berberine,evodiamine,and rutaecarpine showed a good linear relationship in 0.0124—0.124,0.0349—0.349 mg/mL,and 0.6—6,0.5—5μg/mL.The average recovery rates were 99.45%,97.69%,98.18%,and 98.46%,respectively.Conclusion The method is of high sensitivity and nice reproducibility,and it could be used for the simultaneous determination of the four ingredients in Wuji Pellet. 相似文献
17.
目的 应用高效液相色谱(HPLC技术,建立复方利血平氨苯蝶啶片中硫酸双肼屈嗪、氢氯噻嗪和氨苯蝶啶含量的同时测定方法。 方法 采用Alltima C18 色谱柱(4.6 mm×250 mm, 5 μm,以乙腈(A和含0.04%庚烷磺酸钠的50 mmol·L-1磷酸二氢铵溶液磷酸调至pH 3.0(B为流动相,梯度洗脱:0~15 min,A-B为12∶88;15~20 min,A-B由12∶88转变为32∶68;20~30 min,A-B为32∶68,流速0.5 mL·min-1,检测波长280 nm。 结果 在本方法中,硫酸双肼屈嗪、氢氯噻嗪和氨苯蝶啶的线性关系良好,线性相关系数(r都大于0.999 2;专属性强,3种成分和药品中其他成分以及强制降解产物之间都有良好的分离度;精密度和稳定性良好,相对标准偏差(RSD都小于2.0%;加样回收率良好,百分回收率在99.90%和102.8%之间。结论 该方法准确、简单、快速,可作为复方利血平氨苯蝶啶片中硫酸双肼屈嗪、氢氯噻嗪和氨苯蝶啶的同时测定。 相似文献
18.
穿心莲片中内酯类成分的“一测多评” 总被引:1,自引:0,他引:1
目的:建立同时测定穿心莲片中穿心莲内酯、新穿心莲内酯、去氧穿心莲内酯、脱水穿心莲内酯的HPLC方法,在此基础上,建立"一测多评"法的方法学考察方式,验证该方法在穿心莲片质量控制中应用的可行性和技术适用性。方法:以穿心莲片中主要成分脱水穿心莲内酯为指标,建立其与穿心莲内酯、新穿心莲内酯、去氧穿心莲内酯间的相对校正因子,并用该校正因子计算穿心莲内酯、新穿心莲内酯、去氧穿心莲内酯的量,对"一测多评"法的计算值与外标法实测值进行比较。结果:建立了穿心莲片中4种内酯类成分"一测多评"法方法学的考察模式;"一测多评"法对不同的色谱柱和仪器的计算值与外标法实测值之间没有显著性差异。结论:同时测定脱水穿心莲内酯、穿心莲内酯、新穿心莲内酯、去氧穿心莲内酯4种内酯类成分的"一测多评"法方法可靠,结果准确,可用于控制穿心莲片的质量。 相似文献
19.
??OBJECTIVE To determine simultaneously seven ingredients(syringin, hydroxysafflor yellow A, rutin, kaempferol-3-O-rutinoside, anhydrosafflor yellow B, cholic acid and hyodeoxycholic acid)content in Sanchen Pills by quantitative analysis of multi-components by single marker(QAMS). METHODS With hydroxy-safflor yellow A as the indexes,calculated the relative correction factor(RCFs) between other 6 components, and which was used to calculate the content of each component, at the same time the contents of the 6 components were determined by the external standard method, and to compare the two METHODS of the calculation results, to verify the feasibility and accuracy of QAMs method. RESULTS No significant difference between the quantitative RESULTS by QAMS and external standard method was observed in 10 samples of Sanchen Pill. CONCLUSION QAMS can be used as a simple and accurate quantitative quality evaluation method for the determination of a variety of ingredients in Sanchen Pills, which provides a new reference for the quality control of Sanchen pill. 相似文献