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OBJECTIVE To prepare Leonurine hydrochloride tablets and evaluate the quality. METHODS The wet granulation technology was adopted ；leonurine hydrochloride was used as the crude drug ，and the types of fillers ，disintegrants，binders and lubricants were screened by single-factor experiments. Combined with orthogonal experiments ，using the cumulative dissolution rate within 15 minutes（using water as dissolution media ）as index ，the proportion of disintegrants ，the mass fraction of binder solution，and the proportion of lubricants were screened and verified. The in vitro dissolution behavior of the prepared Leonurine hydrochloride tablets （dissolution media were hydrochloric acid solution of pH 1.2，acetic acid-sodium acetate solution of pH 4.5， phosphate buffer solution of pH 6.8，water），tablet appearance ，hardness，friability and content uniformity were tested according to the general principles in 2020 edition of Chinese Pharmacopoeia （part Ⅳ）. RESULTS The optimal formulation of Leonurine hydrochloride tablets included leonurine hydrochloride crude drug of 500 mg，dextrin of 9 250 mg，crosslinking polyving y- pyrrolidone of 200 mg，magnesium stearate of 50 mg，1％ hydroxypropyl methyl cellulose solution of 4 mL. The average 15-minute cumulative dissolution rate of the three batches of tablets was 81.25％（RSD＝1.12％，n＝3）. In above 4 dissolution media，the dissolution equilibrium of prepared tablets could be reached within 30 minutes，and the cumulative dissolution rates exceeded 85％. The prepared tablets had uniform beige in color ，smooth surface ，complete edge ，no mottle ，spot，foreign matter ， etc.，hardness of 57.3 N（n＝6），weight loss rate of 0.15％. The content uniformity was in accordance with relevant provisions in 2020 edition of Chinese Pharmacopoeia （part Ⅳ）. CONCLUSIONS Leonurine hydrochloride tablets are successfully prepared ， and the quality comply with relevant regulations.
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Objective To develop and validate a high performance liquid chromatography coupled with electrospray tandem mass spectrometry (HPLC-ESI-MS/MS) method for simultaneously qualitative and quantitative determination of nine major bioactive components (stachydrine hydrochloride, leonurine hydrochloride, paeoniflorin, ferulic acid, liquiritin, lobetyolin, verbascoside, atracylenolide I, and polyporenic acid C) in Bazhen Yimu Pills (BYP). Methods The chromatographic separation was performed on an Waters Atlantis T3 column (150 mm × 4.6 mm, 3.0 μm) with a gradient elution of methanol and 0.1% formic acid in water at a flow rate of 0.5 mL/min, and the injection volume was 10 μL. The nine major bioactive components were detected using an electrospray ionization source in negative ionization mode (ESI-) and quantified by multiple reaction monitor (MRM) scanning at the same time. Results The linear ranges of stachydrine hydrochloride, leonurine hydrochloride, paeoniflorin, ferulic acid, liquiritin, lobetyolin, verbascoside, atracylenolide I, and polyporenic acid C were 0.04-40.00 μg/mL (r = 0.999 2), 0.04-40.00 μg/mL (r = 0.999 3), 1.0-100.0 μg/mL (r = 0.999 1), 0.2-20.0 μg/mL (r = 0.999 6), 0.2-20.0 μg/mL (r = 0.997 5), 0.05-5.00 μg/mL (r = 0.999 4), 0.1-10.0 μg/mL (r = 0.999 4), 0.1-10.0 μg/mL (r = 0.999 2), 0.1-10.0 μg/mL (r = 0.999 2), and the average recoveries were 99.7% (RSD = 0.52%), 98.1% (RSD = 0.64%), 98.5% (RSD = 1.08%), 101.5% (RSD = 1.12%), 99.5% (RSD = 0.39%), 98.4% (RSD = 0.74%), 99.1% (RSD = 0.91%), 101.2% (RSD = 0.54%), and 100.1% (RSD = 0.47%), respectively. The content of nine batches of the nine major bioactive components were 0.423-0.752, 0.505-0.722, 0.613-1.300, 0.102-0.184, 0.195-0.255, 0.021-0.035, 0.034-0.072, 0.039-0.063, and 0.051-0.095 mg/g, respectively. Conclusion The developed method is simple, specific, and sensitive, and it can be applied for the determination of nine major bioactive components and the quality control of BYP collected from different production batches.
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To build an evaluation standard for quality of Leonuri Herba standard decoction. 13 batches of Leonuri Herba standard decoction with different quality were prepared. The contents of leonurine hydrochloride and stachydrine hydrochloride were determined; then the transfer rate and the extract rate were calculated and pH value was measured; and HPLC fingerprint method was established for analysis. The results of 13 batches of samples revealed that the transfer rate of leonurine hydrochloride and stachydrine hydrochloride was 30.0%-53.4% and 67.0%-82.6%, respectively; the extract rate was 12.1%-18.3% and the pH value was 5.87-6.22. Moreover, 12 common chromatographic peaks were determined based on fingerprint by using Similarity Evaluation System for Chromatographic fingerprint of Traditional Chinese Medicine (2012A). The similarity of 13 batches of samples was analyzed and compared, and the results showed that the similarity was higher than 0.9. In this study, the preparation method for Leonuri Herba decoction was standard, with high similarity in fingerprint, showing high precision, stability and repeatability in fingerprint analysis. Thus, this study can provide a reference for the quality control of Leonuri Herba dispensing granules.
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Objective To study the difference ofLeonurus japonicus germplasm resources and provide good materials for breeding.Methods Totally 20 wildLeonurus japonicus germplasm resources from different places of China were collected. Experiment was conducted in homogeneous garden in Quzhou City of Zhejiang Province. Phenological phase, cold endurance and habitat adaptability were observed; the plant height, fresh weight and dry weight in early flowering were measured; the contents of stachydrine hydrochloride and leonurine hydrochloride were determined in early flowering and out-of-season cultivation.Results Considering the habitat adaptability, dry plant weight in early flowering, the contents of stachydrine hydrochloride and leonurine hydrochloride separately in early flowering and out-of-season cultivation, it was believed that the germplasms from Linbao County, Sheqi County in Henan Province and Guidong County in Hunan Province were better, in which Linbao germplasm was the best: the dry plant weight was 30.6 g, the content of stachydrine hydrochloride and leonurine hydrochloride were 1.31% and 0.19% respectively in early flowering, and were 3.44% and 0.37% respectively under anti-season cultivation, and it can be well adapted in Zhejiang Province.Conclusion The germplasm ofLeonurus japonicas from Lingbao can be the best materials for breeding.
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To establish the quantitative method of stachydrine hydrochloride and leonurine hydrochloride in the preparations of Leonuri Herba. The contents of stachydrine hydrochloride and leonurine hydrochloride in the preparations of Leonuri Herba were determined by HPLC-MS. The chromatographic column was Waters XBridge Amide(4.6 mm×250 mm,5 μm). The mobile phase was acetonitrile-0.1% formic acid in gradient mode,at the flow rate of 1.0 mL• min⁻¹,with the split ratio of 1∶4. MS conditions for the ESI ion source,positive ion mode,selective ion scan(SIM) of stachydrine hydrochloride(m/z 144.0) and leonurine hydrochloride(m/z 312.0) was measured. The linear ranges of stachydrine hydrochloride was 0.562 8-281.4 μg•L-1（r=0.999 8）. The linear ranges of leonurine hydrochloride was 0.521 2-260.6 μg•L-1（r=0.999 8）. The method is accurate,simple,and reliable,and can be used to determine the contents of stachydrine hydrochloride and leonurine hydrochloride in the preparations of Leonuri Herba.