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Objective To establish a RP-HPLC method for simultaneously determining berberine hydrochloride, baicalin, emodin and chrysophanol in Sanhuang tablets. Methods The analysis was performed on an Thermo Hypersil GOLD aQ column (250 mm×4.6 mm, 5.0 μm) with gradient elution of methanol and 0.1％orthophosphoric acid at the flow rate of 1.0 ml/min. The column temperature was 30 , and the detection wave℃length was 254 nm. Results The peaks of berberine hydrochloride, baicalin, emodin and chrysophanol were successfully separated from each other. The liner ranges of calibration curves were 0-0.6348 μg (r=0.9999), 0-1.0172 μg (r=0.9999), 0-0.8024 μg (r=0.9999), 0-0.9672 μg (r=0.9999). The average recoveries (n=9) were 101.03％, 99.81％, 99.35％, 99.54％, respectively. The limits of quantification (LOQs) were 0.0363, 0.0210, 0.0497, 0.0793 mg/g, respectively. The sample solution was stable within 24 h, the RSD (n=5) were 0.48％, 0.56％, 0.68％, 0.49％, respectively. The robustness was investigated by varying the conditions of column temperature (± 1 ℃) and flow rate (± 0.1 ml/min), with the RSD s 0.57％ and 0.42％, 0.44％ and 0.65％, 0.74％ and 0.29％, 0.46％ and 0.56％, respectively. The contents of berberine hydrochloride, baicalin, emodin and chrysophanol in twelve samples were 4.6303-5.5866, 14.5514-18.8189, 0.1711-2.7984, 0.5299-2.9254 mg/tablet, respectively. Conclusion The establish method is validated to be suitable for quality control of Sanhuang tablets.
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AIM To establish an HPLC method for the simultaneous content determination of berberine hydrochloride,baicalin,baicalein,wogonin,aloe emodin,rhein,emodin,chrysophanol,physcion in Sanhuang Tablets (Rhei Radix et Rhizoma,Scutellariae Radix,berberine hydrochloride).METHODS The analysis of methanol extract of this drug was performed on a 35 ℃ thermostatic Waters sunfire C1s column (4.6 mm ×250 mm,5 μm),with the mobile phase comprising of methanol-acetonitrile-0.1％ phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 254 nm.RESULTS Nine constituents showed good linear relationships within their own ranges (r ＞ 0.999 0),whose average recoveries were 99.03％-100.03％ with the RSDs of 0.63％-1.07％.The contents of various constituents in ten batches of samples demonstrated obvious differences.CONCLUSION We should pay attention to the unstable quality of Sanhuang Tablets.
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The qualitative analysis method of ultra performance liquid chromatography tandem quadrupole time of flight mass spectrometry (UPLC-Q-TOF-MS/MS) was established for the chemical constituents in Sanhuang tablets. Waters ACQUITY BEH C₁₈ (2.1 mm×100 mm, 1.7 μm) column was used with 0.1% formic acid solution (A)-0.1% formic acid acetonitrile (B) as the mobile phase for gradient elution. The flow rate was 0.2 mL•min⁻¹; the sample volume was 1 μL and the column temperature was 30 ℃. The high-resolution quadrupole time-flight mass spectrometry was used as detector with electrospray ion source in both positive and negative models, and the dry gas temperature was 325 ℃. Based on the analysis of mass spectrometry and literature reports, 38 compounds were confirmed, including 1 alkaloid, 1 dianthrone compound, 6 tannins, 7 anthraquinone glycosides, 6 anthraquinones and 17 flavonoids. Liquid chromatography-mass spectrometry method is simple, reliable and rapid to identify the chemical compositions of Sanhuang tablets, and it is helpful to reveal its chemical constituents and pharmacodynamic substances.
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Objective: To establish high performance liquid chromatography (HPLC) fingerprints of Siji Sanhuang Tablets (SST) and study the characteristic peaks identification and preparations-medicinal materials peak pattern matching. Methods: Similarity on 10 batches of SST from three manufacturers was estimated, and peak pattern matching of the original medicine was conducted. Sample extraction with methanol in ultrasonic condition (100 kHz, 30 min, 25℃) was carried out. HPLC-Diode Array Detector methods were developed to determine, detection wave length was set at 254 nm, HPLC mobile phase consisted of methanol-0.1% phosphoric acid aqueous solution (gradient elute), volume flow-rate was delivered at 0.8 mL/min, and column temperature was kept at 25℃. Similarity measures such as included angle cosine and correlation coefficient were tested. Ten batches of samples were analyzed by SPSS 16.0. Results: The results showed that 19 common peaks were defined, the peaks No. 1, 2, 4, 17, and 18 were geniposide, berberine hydrochloride, baicalin, emodin, and chrysophanol, respectively, and peak pattern matching showed that SST had 11, 6, 2, and 1 matching peaks with Rhei Radix et Rhizoma, Scutellariae Radix, Gardeniae Fructus, and Phellodendri chinensis Cortex, respectively. The peak No. 9 belonged to Rhei Radix et Rhizoma and Scutellariae Radix. The fingerprint similarity among the samples were all over 0.9. All the samples were classified into three categories. Conclusion: Peak matching fingerprints of preparations-medicinal materials established provide the effective methods for the identification and the quality control of SST.
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AIM:To determine the contents of berberine hydrochloride,palmatine hydrochloride and rhaponticin in Sanhuang Tablets(Radix et Rhizoma Rhei,berberine hydrochloride,extract of Radix Scutellariae) by RP-HPLC. METHODS:RP-HPLC method with Shimadzu TM column(250 mm?4.6 mm,5 ?m) was used. The gradient elution mixture mobile phase consisted of acetonitrile and 0.05% Lauryl sodium sulfate(0.1% phosphoric acid). The flow rate was 1.0 mL/min. The detection wavelength was set at 334 nm. The temperature of column was at 25 ℃. RESULTS:The calibration curves of berberine hydrochloride,palmatine hydrochloride and rhaponticin were linear within the ranges of 0.05-1.04 ?g(r=0.999 9),0.02-0.49 ?g(r=0.999 8),0.05-1.02 ?g(r=0.999 9),respectively. The average recoveries (n=6) were 98.7%,97.2%,99.3%,respectively. CONCLUSION:The method of the operation is accurate,reliable and can be used to control the quality of Sanhuang Tablets.
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Objective: To establish the assay of berberine hydrochloride for Sanhuang Tablets (Radix et Rhizoma Rhei, Extractum Scutellariae and berberine hydrochloride). Methods:The HPLC with a KF C 18 column (250mm?4.6mm,10?m) was used. Acetonitrile-0.05 mol?L -1 triethylamine buffer solution (adjusted pH to 3.0 with conc. H 3PO 4) (35∶65) was used as mobile phase. The flow rate was 1.0mL?min -1 , and the detection wavelength was at 347nm. Results: The method has a good linear dependuce. The average recovery of loading sample was 98.21% with RSD 1.01%. ( n =9). Conclusion: The method is convenient for a good resolution and can be used for the quality control of Sanhuang Tablets.
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Objective: To establish a method for the determination of berberine in Sanhuang Tablets. Methods: By means of colorimetry the complex was determined by combining picric acid and berberine hydrochloride. Results: The method is reproducible. The average recovery was 103.3%. Conclusion: The method can be used for content determination of berberine in Sanhuang Tablets.