Determination of monosaccharide composition of polysaccharide and free monosaccharides in Cistanches Herba by ion chromatography-integral pulsed amperometry / 药学学报

Polysaccharides and free monosaccharides are important active components in Cistanches Herba, which have functions of anti-aging and immunological activity regulation. The study of monosaccharide composition in polysaccharide and free monosaccharide can lay a foundation for the study of primary structure, spatial structure of Cistanche polysaccharide and biological activity of Cistanches Herba. In this study, a method of water extraction and alcohol precipitation was used to extract Cistanche polysaccharide. Trifluoroacetic acid was selected as the hydrolytic acid for polysaccharide hydrolysis. An orthogonal experimental method is established. Three levels of acid concentration, hydrolysis temperature and hydrolysis time were selected to investigate the optimal hydrolysis condition. The optimal hydrolysis condition was 0.08 mol·L-1 trifluoroacetic acid hydrolysis at 100 ℃ for 3 h. The free monosaccharides of Cistanches Herba were extracted by water extraction. The established ion chromatogram integrated pulsed amperometry method can efficiently separate 11 monosaccharides in a short time. The method has good repeatability and high sensitivity, methodological experiment results meet the requirements of quantitative determination. It can accurately determine the monosaccharide composition of Cistanche polysaccharide and free monosaccharide content. Ion chromatography does not require derivatization operation and the pre-treatment steps are simple. This method can measure fructose, but PMP derivation-HPLC method can't. The monosaccharide composition of Cistanche polysaccharide include fucose, arabinose, rhamnose-galactose, glucose, xylose, mannose, fructose, ribose and glucuronic acid, among which the contents of glucose and fructose are relatively high. The free monosaccharides in the water extract of Cistanches Herba include glucose, fructose and mannose.

Quality Analysis and Suggestion for Ginkgo Folium Tablets and Ginkgo Folium Capsules / 中国实验方剂学杂志

Objective:To conduct quality evaluation of Ginkgo Folium preparations by analyzing the national evaluation sampling test results， analyze the quality differences， and put forward suggestions for the improvement of quality standards and market supervision. Method:The contents of total flavonol glycosides and terpene lactones in Ginkgo Folium tablets and Ginkgo Folium capsules were determined according to the methods of determination in the 2015 edition of Chinese Pharmacopoeia （the first volume）， and the contents of free flavonoids （quercetin， kaempferide and isorhamnetin） and sophoricoside in Ginkgo Folium preparations were determined according to related supplementary testing method of Ginkgo Folium tablets and Ginkgo Folium capsules issued by National Medical Products Administration. The quality differences of Ginkgo Folium preparations from different batches and different manufacturers were compared according to the contents of total flavonol glycosides， terpene lactones， free flavonoids and sophoricoside in 328 batches of Ginkgo Folium tablets and Ginkgo Folium capsules manufactured by 48 enterprises. Result:Quality of 328 batches of Ginkgo Folium tablets and Ginkgo Folium capsules was in accordance with the standard， but the contents of terpene lactones and total flavonol glycosides were all distributed in a wide range， and the quality of samples varied greatly among different enterprises. Conclusion:It is recommended that each enterprise should optimize the production process and strictly control the raw materials to ensure the consistency between different batches of samples.

Relative molecular weight determination of astragalus polysaccharides for injection / 药学学报

To determine relative molecular weight of astragalus polysaccharides (APs), we used Shodex GS620 gel permeation chromatographic column and differential refraction detector (GPC-RI) with dextran as a reference. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and GPC combined with multi-angle laser light scattering detection (GPC-MALLS) were also used．GPC-RI measure showed four peaks of APs, with the Mw of 1 380 000, 231 000, 18 000, and 480, respectively. Three main peaks were found by GPC-RI-MALLS with the Mw as 1 148 000, 180 000, and 43 000, respectively. Strong signals in 155 000 and 18 000 were detected by MALDI-TOF-MS, which also indicated the sugar moieties of the APs as hexoses. From our study, we found that the GPC-RI method with universal correction is most suitable for Mw determination of the APs. Nevertheless, the three methods should be combined and contrasted with each other to obtain accurate information in research of polysaccharides from Chinese medicine.

Screening of multiple pesticide residues in Jinyinhua Formula Granules / 中国中药杂志

To evaluate the pesticide residue risk of Jinyinhua Formula Granules( made from Lonicerae Japonicae Flos) used in the market preliminarily,20 samples of Jinyinhua Formula Granules from 5 manufactures were collected randomly through the national evaluative sampling test program. Totally 262 pesticides( involving 270 chemical monomers) with monitoring significance to traditional Chinese medicinal materials were detected. Samples were extracted by high speed homogenate with acetonitrile as solvent. And their residues were analyzed by GC-MS/MS and LC-MS/MS in MRM mode. No less than 2 groups of characteristic ion pairs were adopted for qualitative detection,and the calibration curve method was used for quantitative detection. The results showed that 20 pesticides were detected in 20 batches of Jinyinhua Formula Granules,with an average of about 9 pesticides detected in every batch,but no restricted pesticide was detected. The detected pesticides were all at the trace level,which was far lower than the limit of the general food standard. Therefore,the safety risk was low in Jinyinhua Formula Granules. In this study,a screening method for pesticide residues in Jinyinhua Formula Granules was established for the first time. The method was accurate and rapid,and the detection indicators were highly targeted. The results could provide theoretical reference for the prevention and control of pesticide safety risks in Jinyinhua Formula Granules and even traditional Chinese medicine formula granules.

Quality assessment of sulfur-fumigated paeoniae alba radix / 中国中药杂志

The samples of sulfur-fumigated Paeoniae Alba Radix acquired both by random spot check from domestic market and self-production by the research group in the laboratory were used to evaluate the effects of sulphur fumigation on the quality of Paeoniae Alba Radix by comparing sulfur-fumigated degree and character, the content of paeoniflorin and paeoniflorin sulfurous acid ester, and changes of the fingerprint. We used methods in Chinese Pharmacopeia to evaluate the character of sulfur-fumigated Paeoniae Alba Radix and determinate the content of aulfur-fumigated paeoniflorin. LC-MS method was used to analyze paeoniflorin-converted products. HPLC fingerprint methods were established to evaluate the differences on quality by similarity. Results showed that fumigated Paeoniae Alba Radix became white and its unique fragrance disappeared, along with the production of pungent sour gas. It also had a significant effect on paeoniflorin content. As sulfur smoked degree aggravated, paeoniflorin content decreased subsequently, some of which turned into paeoniflorin sulfurous acid ester, and this change was not reversible. Fingerprint also showed obvious changes. Obviously, sulfur fumigation had severe influence on the quality of Paeoniae Alba Radix, but we can control the quality of the Paeoniae Alba Radix by testing the paeoniflorin sulfurous acid ester content.