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OBJECTIVE:To establish the method for the rapid determination of stilbene glycoside in Shouwu pills. METH-ODS:HPLC method was used to determine the content of stilbene glycoside in Shouwu pills(as measured value). The determina-tion was performed on ODS-C18 column with mobile phase consisted of acetonitrile-water(25:75,V/V)at the flow rate of 0.8 mL/min. The detection wavelength was set at 320 nm,and the column temperature was 30 ℃. The sample size was 10 μL. The partial least square method-near infrared diffuse reflectance spectrophotometry was used to establish quantitative calibration model for pre-dicting the content of stilbene glycoside in Shouwu pills. According to measured value,76 calibration set samples and 24 validation set samples were collected. Standard normalization method and first-order derivative method combined with Savitzky-Goly filter method were used for spectrum pretreatment. The optimal band ranged 9000-4150 cm-1,and main component factor was 12. RE-SULTS:The content determination method of stilbene glycoside in Shouwu pills was in line with the requirements. The correlation coefficients,the root-mean-square error of calibration,the root-mean-square error of predication and the root-mean-square error of cross-validation(RMSECV)of the quantitative calibration model were 0.99190,0.0201,0.0236 and 0.07629. There was no sta-tistical significance between predicted value and measured value(P>0.05). CONCLUSIONS:The method is accurate,stable and simple,and can be used for rapid determination of stilbene glycoside in Shouwu pills.
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Objective To optimize the matrix prescription and preparation technology of compound pyocutaneous gels. Methods Use the method of L9(34 ) orthogonal test, take the Carbopol-940 quantity, pH, glycerol and ethanol as factors,and take viscosity, pH value, appearance properties, temperature resistance as the comprehensive evaluation index, and compare the effects of stewing, centrifugal and ultrasound methods on removing bubbles in the gel. Ultimately determine the optimum preparation process. Results The best matrix prescription of compound pyocutaneous gels is as follows: carbopol-940 1.4%, 10% sodium hydroxide solution 3.3%,glycerol 2.3%,ethanol 6%;the best way to remove bubbles is centrifugation,with rotation rate at 3 000 r?min-1 for 10 min. Conclusion The selected matrix formulation is simple and feasible, the preparation technology is stable and reliable with good reproducibility, and can be used for the preparation of compound pyocutaneous gel.
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Objective To determine the moisture content in Polygoni multiflori Radix rapidly by near-infrared spectroscopy. Methods The moisture content of the samples were determined by oven drying method and the near-infrared spectrum data were collected by near-infrared spectroscopy.The quantitative test model of moisture content in Polygoni multiflori Radix was established by chemometrics methods and was validated with validation samples. Results The correlation coefficients, root-mean-square error of calibration (RMSEC), root-mean-square error of predication (RMSCP) and the root-mean-square error of cross-validation ( RMSECV ) of the calibration model was 0. 984 75, 0. 161, 0. 181 and 0. 471 64, respectively.The absolute deviation of the analytical and predictive values of 21 validation samples was -0.35%-0.28%, and the average recovery was 99. 87%. Conclusion Near-infrared spectroscopy can be used to determine the moisture content of Polygoni multiflori Radix rapidly and accurately.
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Objective To study the influence of climate, geographical environment and harvesting time on contents of schaftoside in Desmodium styracifolium Herba. Methods Content of schaftoside in Desmodium styracifolium Herba was determined by using HPLC. ODS-C18 column (4. 6 mmí250 mm,5 μm) was used, the mobile phase was methanol-water (3268), the detection wavelength was 272 nm, the flow rate was 0. 5 mL·min-1, and the column temperature was 35℃. Results The climate type, amount of precipitation, average temperature, duration of sunshine, geographical environment of different province had significant impacts on the content of schaftoside in Desmodium styracifolium Herba. Conclusion Subtropical monsoon climate, temperature from 25 ℃ to 32 ℃, sunshine time of 10 h per day and the average annual rainfall of 1 942 mm are suitable for growth of Desmodium styracifolium. The content of schaftoside in samples cultivated from Guangxi Province is higher than that cultivated from Guangdong Province and Hainan Province. The schaftoside content of sample cultivated in July is higher than that cultivated in other months.
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Objective To determine the moisture in Huodan pills by near-infrared spectroscopy. Methods At the beginning,water content of 174 samples were determined and all data of samples about near-infrared spectrum were collected. And then all the data were pretreated by first-derivative and Savitzky-Golay filter. At last,the NIR quantitative model for moisture in huodan pills was established by partial least squares regression and validated by the validation set. Results The correlation coefficients,the root mean square error overall of calibration, that of cross validation of the calibration model was 0. 988 17, 0. 103,and 0. 326 16,respectively. The root mean square error overall of prediction and the average recovery of validation was 0. 217 and 98. 02%. Conclusion The NIR spectroscopy analysis model is steady,accurate and reliable,which can be used to detecte moisture content of huodan pills.
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<p><b>OBJECTIVE</b>To establish a near-infrared spectroscopy quantitative model for rapid determination of the patchouli alcohol content in Pogostemon cablin.</p><p><b>METHOD</b>The gas chromatography was adopted for determining the content of patchouli alcohol content in 102 batches of P. cablin samples. Their near-infrared spectrograms were collected and preprocessed by standard normal variate and the first derivative of Savitsky-Golay. The quantitative model of patchouli alcohol content was established by the partial least squares regression analysis.</p><p><b>RESULT</b>According to the correction model established in this study, the root-mean-square error of calibration, the root-mean-square error of prediction and the root-mean-square error of cross-validation of the calibration model for Patchouli alcohol were 0.991 10, 0.012 9, 0.012 8 and 0.033 15, respectively.</p><p><b>CONCLUSION</b>The near-infrared spectroscopy quantitative model established in this study is stable, accurate and reliable for the rapid determination of the content of patchouli alcohol in P. cablin.</p>
Assuntos
Cromatografia Gasosa , Métodos , Lamiaceae , Química , Sesquiterpenos , Espectroscopia de Luz Próxima ao Infravermelho , MétodosRESUMO
OBJECTIVE:To establish RP-HPLC fingerprints of Desmodium styracifolium and its preparations in order to provide basis for the quality evaluation of them.METHODS:The separation was performed on ODS-C18(250 mm?4.6 mm,5 ?m) column with mobile phase consisted of methanol-20% phosphoric acid(gradient elution).The detection wavelength was set at 360 nm and flow rate was 1.0 mL?min-1.Column temperature was set at 25 ℃.The RP-HPLC fingerprint of D.styracifolium and its preparations were recorded.RESULTS:There were 13 common peak in RP-HPLC fingerprint of D.styracifolium and its preparations.CONCLUSION:The method is accurate,stable and reproducible for basis of quality evaluation and RP-HPLC finger print of D.styracifolium and its preparations.