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Objective To develop an HPLC method for the determination of ginsenoside Rb1 in Jupizhuru decoction,and de-termine the amount of ginsenoside Rb1 in 10 batches of Jupizhuru decoction composed of different batch herbs. Methods The HPLC analysis was carried out on a Phenomenex Luna C18 column with column temperature at 30℃,flow rate 1.0 ml/min,detection wave-length 203 nm and mobile phase acetonitrile and 0.1%phosphoric acid by gradient elution. Results The method was found to be lin-ear within the ranges of 5-500μg/ml(r=0.9999),and the average recovery of ginsenoside Rb1 was 95.5%(RSD 1.77%,n=6). Con-clusion The determination method is suitable for the quality control of ginsenoside Rb1 in Jupizhuru decoction.
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Objective To find a new method for quality control of polysaccharides by establishing the fingerprint profiles of polysaccharides extracted from Guifu Dihuang Wan. Methods The polysaccharides extracted from Guifu Dihuang Wan were hydro-lyzed partially under appropriate hydrolysis condition with acid,and the fingerprint profiles of the hydrolyzates was obtained by HPLC. Microsoft Excel 2002 was applied for calculating the similarity of fingerprint profiles,and informatton analysis of these profiles was performed by a software for evaluating fingerprint profiles of traditional Chinese medicine. Results Fingerprint profiles of the hydroly-zates of polysaccharides from 10 of Guifu Dihuang Wan products,produced by different manufacturers,were obtained. It was observed that the similarity of eight products was greater than 0.99,while the similarity of the other two was 0.92 and 0.94,respectively. Con-clusion This method is technically feasible for the quality control of polysaccharides from Guifu Dihuang Wan.
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Objective To develop a LC-MS/MS method for the quantification of empagliflozin(EPLZ)impurity X(EPLZ-X) in EPLZ pharmaceutical product. Methods Isocratic chromatographic separation was performed on a Thermo BDS C18 column(4.6 mm × 100 mm,2.4mm). The mobile phase consisting of acetonitrile-water(75∶25,V/V)was eluted at a flow rate of 0.7 ml/min. ESI source was applied and operated in the positive ion mode. multiple reaction monitoring(MRM)mode with the transitions of m/z 785→m/z 475 and m/z 785→m/z 418 were used to quantify the EPLZ-X. Results The method was linar in the concentration range from 0.5 to 100.6 ng/ml. The limit of quantification was 0.5 ng/ml. The intra-and inter-day precision values were both below 11.8%,and accuracy was within ±2.5%in all quality control samples. The average recovery was 105.1%、109.8%and 102.6%,respectively. Conclusion The method provides a sensitive and specific means for the determination of EPLZ-X in EPLZ pharmaceutical substances and completely meets the requirement of European Medicines Evaluation Agency(EMEA)(a limit of not more than 60×10-6 g for the mutagenic impurity EPLZ-X).
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OBJECTIVE:To establish a method for the determination of 7 residual solvents(ethanol,n-hexane,benzene,tolu-ene,xylene,styrene,divinylbenzene)in Liuwei dihuang glycoside. METHODS:The column was DB-624 capillary column,carri-er gas was nitrogen,flow rate was 5.0 ml/min;detector was a hydrogen flame ionization detector with temperature of 250 ℃(pro-grammed temperature);equilibrium temperature was 80 ℃,sample loop temperature was 90 ℃,and transfer line temperature was 100 ℃;the equilibrium time of vial heating was 30 min,sample loop filling time was 0.05 min,injection time was 1.0 min;the carrier gas pressure was 95 kpa,and the vial pressure was 60 kpa. RESULTS:The linear range was 25-500 μg/ml for ethanol(r=0.998 7),0.025-10μg/ml for n-hexane(r=0.998 8),0.025-10μg/ml for benzene(r=0.999 9),0.1-40μg/ml for toluene(r=1.000 0),0.25-100 μg/ml for xylene(r=0.999 9),0.5-500 μg/ml for styrene(r=1.000 0) and 0.5-500 μg/ml for divinylbenzene (r=1.000 0);RSDs of precision,stability and reproducibility tests were lower than 4%;recoveries were 99.60%-102.70%(RSD=1.08%,n=9),90.70%-100.30%(RSD=4.51%,n=9),100.10%-109.80%(RSD=3.82%,n=9),99.50%-110.00%(RSD=4.40%,n=9),100.00%-109.10%(RSD=3.50%,n=9),93.40%-102.30%(RSD=3.73%,n=9) and 99.70%-101.70%(RSD=0.79%,n=9),respectively;the low limits of detection were 1.000,0.025,0.025,0.025,0.100,0.025,0.250 μg/ml respectively. CONCLUSIONS:The method is simple,stable and reproducible,and can be used for the determination of residual solvents(etha-nol,n-hexane,benzene,toluene,xylene,styrene,divinylbenzene)in Liuwei dihuang glycoside.
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This study was aimed to explore the impact of activated carbon adsorption modified by different concentrations of nitric acid and ammonia,in order to examine the impact on adsorption of mannotriose by modified activated carbon.The activated carbon was processed by different concentrations of nitric acid and ammonia.And then,the adsorption capacity of benzene,iodine,methylene blue and the purification effects on mannotriose were measured.The results showed that the active carbon modified by nitric acid and ammonia had some changes of adsorptions for methylene blue,iodine and benzene.The purification effect of mannotriose with nitric acid-modified activated carbon was declined.The purification effect of mannotriose with ammonia-modified activated carbon was increased.It was concluded that the pore structure of activated carbon had been changed by nitric acid and ammonia.The adsorption capacity of nitric acid modified active carbon to mannotriose was declined.However,the adsorption capacity of ammonia modified active carbon to mannotriose was increased.It showed that ammonia modified active carbon was suitable for the purification of mannotriose.And the adsorption capacity of iodine reflected the adsorption capacity of mannotriose by active carbon.
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Objective To prepare cysteamine group substitutes of catechin compounds from Weimaining. Methods After thiolased by cysteamine, Weimaining was subjected to the open column chromatography on C18, and subsequently to the semi-preparative high performance liquid chromatograph (HPLC) to prepare the cysteamine group substitutes of catechin compounds. Results Compounds 4β-(2-aminoethylthio)catechin, 4β-(2-aminoethylthio)epicatechin, and 4β-(2-aminoethylthio) epicatechin-3-O-gallate were obtained, and their purities were above 95%. Conclusion The method is simple and easy, and provides a reference for the preparation of the cysteamine group substitutes of catechin compounds.
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Tanshinone II A, which was known unique to the salvia, was separated and purified by silica gel column chromatography and recrystallisation from an ethyl acetate-soluble portion (the anti-inflammatory active portion) of ethanol extract of Periploca forrestii. The diterpenoid quinone was obtained from the Periploca for the first time.
Subject(s)
Diterpenes , Drugs, Chinese Herbal , Periploca , Chemistry , QuinonesABSTRACT
<p><b>OBJECTIVE</b>To establish a method for content determination of polysaccharides in Periplocaforrestii.</p><p><b>METHOD</b>The conversion coefficient of P. forrestii. polysaccharide to glucose was obtained by refined polysaccharides, and then the content of crude polysaccharides was determined by sulfuric-phenol method.</p><p><b>RESULT</b>The content of crude polysaccharides in P. forrestii. was 54.68% (RSD 3.0%, n = 6), and the average recovery was 101.7% (RSD 6.0%, n =6).</p><p><b>CONCLUSION</b>The method was simple, rapid, and accurate.</p>
Subject(s)
Chromatography, High Pressure Liquid , Methods , Colorimetry , Drugs, Chinese Herbal , Chemistry , Flowers , Chemistry , Periploca , Chemistry , Phenols , Polysaccharides , Spectroscopy, Fourier Transform Infrared , MethodsABSTRACT
AIM To investigate the structures and immunomodulation activity of four homogeneous polysaccharides: LBP 1a-1, LBP 1a-2, LBP 3a-1 and LBP 3a-2 isolated from Lycium barbarum L. brought from Zhongning County, Ningxia Province. METHODS Their molecular weights, sugar component (constituents) and their linkages were determined by gel permeation chromatography, acid hydrolysis, periodate oxidation and NMR spectrum. The activity of immunomodulation was evaluated with splenocyte proliferation by ［3H］-TDR incorperation, in vitro. RESULTS Four polysaccharides with molecular weights 11.5×104, 9.4×104, 10.3×104 and 8.2×104, were shown to enhance splenocyte proliferation induced by ConA. LBP 1a-1 and LBP 1a-2 were α-(1→6)-D-glucans. LBP 3a-1 and LBP 3a-2 were found to be α-(1→4)-D-polygalacturonans. CONCLUSION The four polysaccharides were first isolated from this plant. Polysaccharides with main chain of α-(1→4)-D-polygalacturonans showed stronger immunomodulation activity.
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Object To isolate the immunoactive polysaccharide from Astragalus mongholicus Bunge and elucidate its chemical structure Methods The polysaccharide was purified from water extracts of A mongholicus by ethanol precipitation, deproteination, selective precipitation with hexadecyltri methylammonium bromide, ion exchange and gel filtration chromatography Its homogeneity and molecular weight were estimated by gel filtration chromatography, the structure was deduced from sugar analysis, methylation analysis, Smith degradation, IR and 13 CNMR spectrophotometry Results A homogeneous polysaccharide A2Nb was obtained with a molecular mass of 360 000 , and composed of D glucose with a major linkage form of ? D (1→4) glucose Side chains were found at 6 O positions once in every 25 glucose residues Conclusion A high molecular weight glucan A2Nb was obtained from A mongholicus for the first time It showed the ability of promoting the proliferation of the splenocytes of mice