RESUMEN
Research on polymer impurities has always been important in the quality control of cephalosporins. Research on polymers in cephalosporins that lack active amino groups on the C-7 side chain has not been reported. Therefore, our study used cefazolin sodium, which is widely used in the clinic, as an example. The polymer in cefazolin sodium and its product "cefazolin sodium pentahydrate for injection" was analyzed by column switching liquid chromatography-high resolution mass spectrometry. Two polymer impurity peaks were detected and the possible structures of these polymers were suggested. Through two-dimensional liquid chromatography, the chromatographic peaks following Sephadex gel chromatography and high-performance gel chromatography were compared to those obtained by reverse high-performance liquid chromatography (HPLC) for cefazolin sodium as reported in the Chinese Pharmacopoeia. The HPLC method proves more suitable for polymer detection than Sephadex gel chromatography and high-performance gel chromatography. The method of polymer detection for cefazolin sodium was established using the method of related substances HPLC as described in the Chinese Pharmacopoeia.
RESUMEN
Objective: To establish a method for determining the content of total polysaccharides in decoction pieces of Polyporus,analyze the content of total polysaccharides in samples with different sources and grades. Method: The relative molecular weight and the polydispersity index of polysaccharides in decoction pieces of Polyporus were measured by a high performance gel chromatography coupled with a multi-angle laser light scattering and refractive index system.Dextran with similar molecular weight as polysaccharides was selected as the reference substance.Orthogonal experiment and single factor tests were used to optimize the pretreatment conditions for the determination of total polysaccharides in Polyporus.Polysaccharides in Polyporus with different areas and grades were determined by anthrone-sulfuric acid colorimetric method at 630 nm. Result: The linearity,stability,precision,repeatability and recovery rate of the established method all reached the standards,respectively.The content of total polysaccharides in samples from different areas ranged from 0.87% to 1.39%.The content of total polysaccharides in samples with different grades was 1.40% for first-grade pieces,1.21% for second-grade pieces, and 1.03% for third-grade pieces. Conclusion: The established method is simple,accurate and reproducible,and it can be used for the determination of polysaccharides in decoction pieces of Polyporus.The content of polysaccharides in samples from different origins varies greatly.The content of polysaccharides in samples with different grades shows a certain regularity.The content of polysaccharides is the highest in the first-grade pieces,followed by the content in the second-grade,and the lowest in the third-grade.The results can provide a reference for formulating limits for the content of total polysaccharides and the grade standard of decoction pieces of Polyporus.
RESUMEN
Objective: To optimize the extraction process of polysaccharide from Codonopsis pilosula and determine the monosaccharide composition and molecular weight distribution, in order to provide the basis for further separation of C. pilosula polysaccharide. Methods: The content of polysaccharide in C. pilosula was determined by phenol sulfuric acid method, the extraction process of polysaccharide was optimized by orthogonal test. C. pilosula polysaccharides were prepared from crude polysaccharides by deproteinization, decoloration, dialysis, and lyophilization, then monosaccharide composition and mean molecular mass of C. pilosula polysaccharides were analyzed by high performance liquid chromatography (HPLC) and high performance gel permeation chromatography (HPGPC). Results: The extraction temperature was 85 ℃, the extraction time was 1.5 h per time, twice, and solid to liquid ratio was 1:12. Under these conditions, the yield of polysaccharides was 22.57%. The polysaccharides were consisted by glucuronic acid, aminogalactose, xylose, and small quantities of mannose, the average molecular mass was 21 498. Conclusion: This study provides a theoretical basis for the classification and activity of polysaccharide from C. pilosula.