ABSTRACT
OBJECTIVE： To investigate the rationality of TLC identification method （3） of （R，S）-epigoitrin in Isatis indigotica stated in 2015 edition of Chinese Pharmacopeia （partⅠ） （later abbreviated as pharmacopeia）， and make some improvements. METHODS： Three batches I. indigotica were collected and prepared into decoction pieces according to the processing method of I. indigotica in pharmacopoeia. TLC identification of （R，S）-goitrin in I. indigotica decoction piece and medicinal material were conducted according to identification method （3） in pharmacopeia （80％ ethanol as solvent for sample treatment， ultrasound extraction）； the rationality of pharmacopoeia method was investigated. Then the method was improved by changing the extraction solvent and pretreatment method （method one： using water as solvent， ultrasound extraction； method two： soaking in water for 1 h， then adding into methanol， ultrasound extraction； method three： the sample was wetted and then dried， using 80％ methanol as solvent， ultrasound extraction） of samples， and the optimal method was verified. According to the optimal method， the TLC identification of （R，S）-goitrin was detected by using chromatographic plates from different manufacturers， under the conditions of low temperature and low humidity （7 ℃， relative humidity 48％） and high temperature and high humidity （35 ℃， relative humidity 75％） respectively，to investigate the durability of the method. RESULTS： According to the method of pharmacopeia， in the chromatograms of decoction pieces， the same color spots appeared at the corresponding chromatographic positions of reference substance， but no corresponding spots appeared in the medicinal material chromatograms. After the samples were treated by three improvement methods， in medicinal material chromatograms， the same color spots appeared in the corresponding chromatographic positions of reference substances. There were single chromatographic spot after medicinal materials were treated with method one， and there were more spots after medicinal materials were treated with method two and three， and method two consumed less time than method three. The results of validation tests and method durability tests showed that after the treatment of I. indigotica and its decoction pieces according to method two， the same color spots appeared in the corresponding positions of the decoction pieces and the medicinal materials chromatograms as those of the control. CONCLUSIONS： The improved TLC identification method is effective， the chromatographic spots are clear， and the repeatability is good.
ABSTRACT
OBJECTIVE:To establish the quality standard for Gentiana scabra dispensing granule. METHODS:TLC was ad-opted to identify G. scabra in the preparation;HPLC was adopted to determine the content of gentiopicroside in the preparation:the column was Dionex C18 with mobile phase of methanol- water(25∶75,V/V)at a flow rate of 1.0 ml/min,the detection wave-length was 270 nm,column temperature was 30 ℃,the injection volume was 10 μl. RESULTS:TLC showed clear spots and good separation. The linear range of gentiopicroside injection volume was 0.302 6-3.026 μg (r=0.999 9);RSDs of precision,stability and reproducibility tests were lower than 2%;recovery was 98.27%-99.56%(RSD=0.68%,n=6). CONCLUSIONS:The estab-lished standard can be used for the quality control of Gentiana scabra dispensing granule.
ABSTRACT
Objective:To set up the HPLC fingerprints of Scutellaria baicalensis collected from different regions and develop a HPLC method for the quantitative analysis of the chief Flavonoids in Scutellaria baicalensis.Methods:The HPLC separation was performed on SHIMADZU VP-ODS column(250mm?4.6mm,5?m),gradient eluted using 0.1% citric acid-acetonitrile solvent system and detected at 276nm and 200nm to 400nm with a DAD detector.The flow rate was 1.0ml/min.The fingerprints of different samples were compared with similarity evaluation software.Results The HPLC fingerprints of Scutellaria baicalensis was set up,in the fingerprints,17common peaks of flavonoids were confi rmed.But the contents of the chief Flavonoids had a big difference,in which the baicalin had the biggest content(18.32%) in cottage Scutellaria baicalensis of Yiyuan County;the baicalein and wogonin had the biggest content(2.31%&0.73%) in wild Scutellaria baicalensis of Northeastern China.Conclusion:This method showed high precision,good repeatability,stability and all of the content were separated well,so it can be useful as the means to assess the quality of Scutellaria baicalensis.