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OBJECTIVE: To identify the main chemical constituents in the extract of deep fried strychnas by UPLC-Q-TOF-MS. METHODS: Agilent SB-C18(2.1 mm×100 mm, 1.8 μm) column was used. Gradient elution was conducted with mobile phase consisting of 0.1% formic acid solution (A) and acetonitrile (B)at a flow rate of 0.2 mL•min-1. The column temperature was maitained at 35 ℃. MS analysis was based on information associated mode (IDA) that positive and negative ions were respectively collected. RESULTS: A total of 31 compounds were identified in deep fried strychnas, of which eight had not been reported as Semen Strychni,and four new compounds were found in the positive and negative ion mode. The main chemical constituents included alkaloids, organic acids, glycosides, etc. CONCLUSION: The method is accurate, reliable, and efficient, and is suitable for rapid identification of the ingredients in deep fried strychnas, which provides a reference for the development and utilization of processed products of Semen Strychni and clarification of its efficacy and material basis.
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Objective Brucine and strychnine monomer reference substance as extremely toxic substance had potential threat during transportation and utilization. In this study we investigated the homogeneity, stability and assignment accuracy of the mixture reference solution of strychnine and brucine, so as to provide reference for the quality control of extremely toxic chemical reference substances for Chinese medicine. Methods Following the assay in Chinese Pharmacopoeia volume I (2015), we prepared the mixture reference solution of brucine and strychnine, and investigated the solvents and the concentration of mixutre reference solution. The stability test lasted for 12 months. F-test was used for heterogeneity assay. Three researchers were involved for collaboration. Results Methanol and chloroform solution were selected as the solvents for the stability test. Results showed the difference was not statistically significant among various mixture solutions. The results of value assignment were 0.14 mg/mL for strychnine (sR = 0.5％)and 0.10 mg/mL for brucine (sR = 1.0％). The stability of mixture solution were better under the conditions of methanol solution at 4 ℃ or -20 ℃. Conclusion The results provide a possible way to develop the mixture solution in place of the monomer reference, and the mixture reference solution is expected for the quality control in the slices of Semen Strychni and its compound preparations.
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OBJECTIVE: To establish the HPLC fingerprint of Semen Strychni by chemometrics and the method of linear calibration using two reference substances (LCTRS). METHODS: The fingerprint of Semen Strychni was established by HPLC, using similarity analysis, 2-dimensional clustering analysis and principal component analysis for quality evaluation. LCTRS was used for identification of chromatographic peak. RESULTS: Fourteen chromatographic peaks were selected as common peaks in the fingerprints of 10 batches of Semen Strychni, and the chromatographic peaks of loganic acid, chlorogenic acid, strychnine and brucine were selected as characteristic peaks. By means of chemometrics evaluation, 10 batches of Semen Strychni were classified by their origins. The precision of predicting retention time by LCTRS was superior to the relative retention time method. CONCLUSION: LCTRS is more accurate for predicting retention time and suitable for more kinds of chromatographic columns than relative retention time method. In addition, the established fingerprint is specific, and can be used for the quality evaluation of Semen Strychni.
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Objective To develop a RP-HPLC method for the determination of Brucine and Strychnine in Semen Strychni and its extractive of total alkaloids. Methods A chromatographic column of Licrospher C18 (4.6 mm×250 mm, 5 μm) was used with the mobile phase of acetonitrile∶0.01 mol/L sodium heptane sulfonate and 0.02 mol/L potassium dihydrogen phosphate mixed with equal amount (adjusted pH to 2.8 with 10% phosphonic acid)=27∶73, detection wavelength at 260 nm, column temperature of 30 ℃ and flow rate of 1 mL/min. Results The calibration curves of Brucine and Strychnine were both in good linearity in the ranges of 0.1-1.0 μg and 0.12-1.2 μg (r=1.000) respectively. The average recovery rates of Brucine and Strychnine were 99.88% (RSD=1.06%) and 100.06% (RSD=0.78%) respectively. Conclusion The method is realiable and accurate, which can be applied to determination of Brucine and Strychnine in Semen Strychi and its extractive.
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Objective:To study the pharmacokinetic process ofbrucine from normal and ultra-micro powder ofsemen strychni in rat serum.Methods:HPLC techniques were used.All pharmacokinetics parameters were calculated with a 3P87 program.Results:The pharmacokinetics results indicated that the normal powder and the ultra-micro powder ofsemen strychni belonged to two compartment open model.The absorb ofbrucine was just several ten minutes, and there was no obvious difference ofTmax between normal powder and ultra-micro powder.This showed that:Brucine was some material that was easily absorbed.But we can find that Cmax increased from(51.13?0.48)?g/L to(69.26?1.40)?g/L after ultra-micro powder preparation which was quite obvious.K,Ka,B and ? had a obvious increase(P
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Objective To establish the RP- HPLC method for the determination of total alkaloids in Semen Strychni and to optimize its extraction conditions by orthogonal design. Methods With strychnine and brucine content as the indexes, ethonal volume, ethonal concentration , pH and extracting time were screened and L9(34) orthogonal test were applied. Results The optimal extraction conditions were as follows: refluxing and extracting with 6- fold 50 % alcohol (pH=5) for 3 times, one hour for each time. Conclusion The optimized condition is the best for the extraction of alkaloids and this increase the availability of Semen Strychni.
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AIM: To investigate the influence of compatibitity in Fengshi Maqian Tablet [ABD group(Semen strychni,Bombyx batryticatus,Herba ephedrae,Scorpio,Rhizoma atractylodis,Radix et Rhizoma glycyrrhizae) E group(Olibanum;Myrrha)]. METHODS: In the use of orthogonal design(5 factors and 2 levels).HPLC method were used to determine the main chemical componets such as strychnine,brucine and ephedrine.And anti-inflammation was adopted as pharmacological experiment. RESULTS: In the inhibitive experiment of granuloma,ABD group was superb to E group.In the tumescence experiment,otherwise. CONCLUSION: The minister,assistant and guide herbs in Fengshi Maqian Prescription had a significant effect on the toxicity of monarch medicines-Semen strychni.
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To assay the quantity of the brucine ingredient in gastric content and hepatic tissues from the patient died of Semen Strychni hainanensi accumulative posioning.With standard brucine and the crude powder of the Semen Strychni hainanensi as control,the brucine ingredients in the above tissues were quantitatively scanned by the capillary elecrophoretic apparatus within the wave length ranging 190～600nm.The contents of the brucine ingredients in the gastric,hepatic tissues and the crude powder of the Semen Strychni sainanensi were 5 83mg/100ml,4 92mg/100g,and 3 07%(w/w)respectively.The high level of the brucine ingredients in the gastric content and the hepatic tissue is the cause of death.