Improvement on Quality Standard of Belladonnae Herba / 中国实验方剂学杂志

ObjectiveTo improve the current standard of Belladonnae Herba in the 2020 edition of Chinese Pharmacopoeia. MethodTaking hyoscyamine sulfate， atropine sulfate and scopoletin as reference substances， and ethyl acetate-methanol-concentrated ammonia（17∶4∶2）as developing solvent， thin layer chromatography （TLC） was applied in the qualitative identification of Belladonnae Herba. The moisture， total ash and ethanol-soluble extract of Belladonnae Herba were determined based on the general principles in the 2020 edition of Chinese Pharmacopoeia （volume Ⅳ）. The contents of hyoscyamine sulfate and scopolamine hydrobromide were analyzed by high performance liquid chromatography （HPLC） with mobile phase of acetonitrile-54 mmol·L-1 phosphate buffer solution （14∶86）， flow rate of 1.0 mL·min-1 and detection wavelength at 210 nm. ResultThe spots in the TLC were clear with good separation and specificity. Hyoscyamine sulfate and scopolamine hydrobromide showed a good linearity with peak area in the range of 0.024 7-0.789 6 g·L-1 （r=0.999 9） and 0.003 9-0.124 0 g·L-1 （r=0.999 9）， the average recoveries of these two ingredients were 100.29% （RSD 1.6%） and 99.04% （RSD 1.4%）， respectively. The limits for moisture， total ash in Belladonnae Herba should be less than 13.0% and the limit for the ethanol-soluble extract should be more than 10.0%. Due to the low content and wide variation of scopolamine hydrobromide， the content of hyoscyamine sulfate should not be less than 0.098%. ConclusionThe established method is simple， specific and reproducible， which can be used to improve the quality control standard of Belladonnae Herba.

Quality standards of Gleditsiae Spina and its decoction pieces / 中国中药杂志

In view of the current inadequate standards for Gleditsiae Spina in the Chinese Pharmacopoeia, this study put forward some new items of the quality standards of Gleditsiae Spina. Thin-layer chromatography(TLC) was performed for identification with the reference substance of taxifolin and the reference material of Gleditsiae Spina as the control. According to the general principles of the Chinese Pharmacopoeia(2020 edition, Vol. 4), the moisture, total ash content, and alcohol-soluble extract of medicinal materials and decoction pieces of Gleditsiae Spina were determined. The content determination method for medicinal materials and decoction pieces of Gleditsiae Spina was established using high-performance liquid chromatography(HPLC), with taxifolin as the quality control index. Based on the determination results of 30 batches of samples of Gleditsiae Spina from different habitats, the draft quality standards of Gleditsiae Spina were developed, which provided suggestions for the revision of the quality standards of Gleditsiae Spina in the Chinese Pharmacopoeia.

Simultaneous Determination of Seven Constituents in Qinggan Lidan Mixture by HPLC / 中国实验方剂学杂志

Objective: To establish an HPLC method for simultaneous determination of geniposide,chlorogenic acid,neochlorogenic acid,cryptochlorogenic acid,isochlorogenic acid A,B and C in Qinggan Lidan mixture,in order to provide references for its quality control. Method: The analysis of methanol extract of this drug was performed on a 35℃ Luna C18 column (4.6 mm×250 mm,5μm),with the mobile phase comprised of acetonitrile-0.4% phosphoric acid flowing at 1.0 mL·min-1 in a gradient elution mode (0-10 min,8%-12%A;10-30 min,12%A;30-60 min,12%-35%A),and the detection wavelengths were set at 238 and 327 nm. Result:Geniposide,chlorogenic acid,neochlorogenic acid,cryptochlorogenic acid,isochlorogenic acid A,B and C were completely separated,and well separated from other constituents. The linear ranges of geniposide,chlorogenic acid,neochlorogenic acid,cryptochlorogenic acid,isochlorogenic acid A,B and C were 0.188-2.355,0.083-1.040,0.074-0.920,0.075-0.940,0.064-0.800,0.076-0.955,0.071-0.888 μg (r ≥ 0.999 0),respectively. The average recoveries were 99.45%,98.45%,99.06%,98.50%,98.16%,101.01%,96.93%,with the RSDs of 0.5%,1.8%,1.3%,2.4%,2.3%,1.6%,1.6%,respectively.The contents of geniposide,chlorogenic acid,neochlorogenic acid,cryptochlorogenic acid,isochlorogenic acid A,B and C were 3.420-3.794,0.835-0.890,1.222-1.275,1.064-1.210,0.377-0.398,0.419-0.464 and 0.362-0.405 g·L-1,respectively. Conclusion:This method can be used for simultaneous determination of muti-ingredients in Qinggan Lidan mixture,and the established method is simple and accurate,with a good reproducibility and high sensitivity. It can be used for the quality control of Qinggan Lidan mixture.

Pharmacokinetic Study of Ocotillol in Rats by LC-MS /MS / 中国药学杂志

OBJECTIVE: To develop an LC-MS /MS method for the quantitative analysis of ocotillol in rat plasma, and study the pharmacokinetic characteristics of ocotillol in rats after oral administration. METHODS: Ocotillol was extracted from plasma sample by protein precipitation. The concentration of ocotillol in plasma was determined by LC-MS/MS and the plasma concentration-time curve and main pharmacokinetic parameters were calculated after a single oral administration of ocotillol at 40 mg•kg-1 to SD rats. RESULTS: Excellent linearity was found between 10 - 240 ng•mL-1. Intra-and inter-day precision values (RSDs) of QC samples were both below 15% and the extraction recoveries of ocotillol from plasma were higher than 84.14%. Double peaks were observed in the mean plasma concentration versus time profile of ocotillol after oral administration. The main pharmacokinetic parameters of ocotillol were as follows: the mean maximum plasma concentration (ρmax) was (156.60 ± 51.84) ng•mL-1 occurring at (0.83 ± 0.26) h post dose, the mean elimination half-time (t1/2) was (8.82 ± 7.56) h, and the mean area under the plasma concentration versus time curve (AUC0-t) was (687.15 ± 144.08) ng•h•mL-1. CONCLUSION: The current data shows that ocotillol is rapidly absorbed in rats after oral administration and slowly eliminated from circulatory blood system, with low plasma exposure. Enterohepatic circulation may contribute to the atypical drug absorption profiles.

Neuroprotective effects of Yiqihuoxue calm wind capsule on ischemic stroke in rats / 中国天然药物

Stroke remains the third leading cause of death and of adult disability worldwide. Vascular occlusion, followed by ischemic cascade, leads to irreversible tissue injury. Recombinant tissue plasminogen activator is the only FDA approved drug for the current treatment of acute ischemic stroke. However, traditional Chinese medicine has a long history and rich clinical experience in the treatment and rehabilitation of ischemic stroke. Using a classical middle cerebral artery occlusion (MCAO) stroke model, we tested the effectiveness of Yiqihuoxue calm wind (YCW) capsule on neurological function, gross pathology and oxidative stress status in MCAO rats. YCW capsule (3.36 and 6.72 g·kg of crude drug) could significantly lower Longa's score and superoxide dismutase (SOD) level, together with less necrotic cells and infarcted area. In addition to elevated MDA and downregulated iNOS expression, YCW capsule exhibited its neuroprotective effects via free radical scavenging and NO inhibition.

Chemical constituents from lipophilic parts in roots of Angelica dahurica cv.Yubaizhi / 中国中药杂志

The chemical constituents from lipophilic parts in the roots of Angelica dahurica cv. Yubaizhi were studied in this paper. The compounds were separated and purified by repeated column chromatographic methods on silica gel and HPLC, and the chemical structures of compounds were determined by spectral data analyses. Thirty-three compounds were obtained and identified as isoimperatorin (1), imperatorin (2), stigmasterol (3), isooxypeucedanin (4), pabulenol (5), psoralen (6), bergapten (7), isodemethylfuropinarine (8), phellopterin (9), osthenol (10), alloimperatorin (11), xanthotoxin (12), xanthotoxol (13), isopimpinellin (14), alloisoimperatorin (15), β-sitosterol (16), oxyalloimperatorin (17), pabularinone (18), 5-hydroxy-8-methoxypsoralen (19), columbianetin (20), heracol (21), isogosferol (22), 2″R-neobyakangelicol (23), byakangelicin ethoxide (24), byakangelicin (25), oxypeucedanin hydrate (26), uracil (27), umbelliferone (28), bergaptol (29), demethylfuropinarine (30), isobyakangelicol (31), oxypeucedanin ethanolate (32), heraclenol (33). Among them, compounds 8, 10, 17, 21, and 30 were obtained from the roots of title plant for the first time.