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Objective To establish the assay method for the total polysaccharide in Pudi Enema.Methods Phenol-sulfuric acid method was used for chromogenic reaction.The content of total polysaccharide was measured by UV spectrophotometry at 488.8 nm.Results The total polysaccharides calibration curve was at the range of 0~22.635 mg/L, with regression function being Y=0.062 06 X-0.003 34(r=0.999 8).The recovery of calycosin was 98.36%(RSD=2.34%).Conclusion This method is sensitive,rapid,accurate and reliable.It can be used to assay the content of total polysaccharide in Pudi Enema.
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OBJECTIVE: To establish the reference standard of melatonin. METHODS: The structure of the reference standard was identified by UV, IR, NMR, and ESI-MS spectrophotometry. The purity was calculated by normalization method and self-contrasted dilution method. Furthermore, loss on drying, residue on ignition, and hygroscopicity were tested. RESULTS: The purity was 99.8% by normalization method and self-contrasted dilution method. COCLUSION: The establishment of reference standards of melatonin can efficiently control the addtion of melatonin into lunctional foods.
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OBJECTIVE: To review the progress in the content assay methods of sulfate polysaccharide drugs. METHODS: By nonsuiting the literature at home and abroad in recent years, the content assay methods of sulfate polysaccharide drugs, including direct staining method, acid-degradation color-development method, photometric titration, liquid chromatography and biopotency, are introduced and compared. RESULTS AND CONCLUSION: The specificity, precision and accuracy, feasibility of practical operation and the instrument cost of the five methods are different. But high performance liquid chromatography method with good specificity, high sensitivity, and accuracy can give more accurate result of the drug content. It is more widely applied in the determination of drug content, so it will be the main method of content assay in the future.
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OBJECTIVE: To develop an HPLC method for simultaneous determination of multiple-components in Hedyotis diffusa Willd. METHODS: The HPLC analysis was carried out on a C18 column (4.6 mm×250 mm, 5 μm) by gradient elution with acetoni-trile-water[both containing 0.1‰ (V/V) acetic acid] as mobile phase at a flow rate of 0.8 mL·min-1, the column temperature at 35°C, and the detection wavelength was set at 238 nm. External standard method and quantitative analysis of multi-components by single marker (QAMS) method were adopted for simultaneous determination of six components in Hedyotis diffusa Willd, respectively. RESULTS: The linear ranges for asperulosidic acid, quercetin-3-O-[2-O-(6-O-E-feruloyl)-β -D-glucopyranosyl]-β-D-glucopyrano-side, kaempferol-3-O-[2-O-(6-O-E-feruloyl)-β-Z) -gfucopyranosyl]-β-D-galactopyranoside, (E)-6-O-p-coumaroyl scandoside methyl ester, (E)-6-O-feruloyl scandoside methyl ester, (Z)-6-O-p-coumaroyl scandoside methyl ester were 2.34-93.50, 2.61-104.33, 0.67-26.69, 3.42-136.84, 0.65-26.07, and 1.10-44.17 μg·mL-1 (r<0.9993), respectively. The RSD values of precision, reproducibility, and sample stability were not more than 2.2%. The average recoveries of the six components were 99.8%-101.1% with RSDs not more than 1.2%. The P values of external standard method and QAMS by paired t-test were greater than 0.05. CONCLUSION: There is no significant difference in the content analysis results of the two methods, which can both used for simultaneous determination of the four iridoids and two flavonoids in Hedyotis diffusa Willd.
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Objective: To establish a HPLC method to determinate the content of rocuronium bromide. Methods: NH2-bonding silica gel was used as the stationary phase. The mobile phase consisted of 0.04 mol/L tetramethyl ammonium hydroxide (pH adjusted to 7.4 by phosphoric acid) and acetonitrile (10:90). The column temperature was 35°C. The detection wavelength was 207 nm. Results: The relation between concentration and peak area was linear in the range of 0.1251-2.0065 mg/ml with r2 of 0.9999. The average recovery rate was 99.9% with RSD of 0.1%. Conclusion: This method is exclusive, sensitive and is reliable for the determination of rocuronium bromide.