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OBJECTIVE To optimize the preparation process of Soft-shelled turtle blood lyophilized powder （STBLP）， and to provide a reference for improving the availability and quality stability of soft-shelled turtle blood （STB）. METHODS STBLP was prepared with vacuum freeze-drying. Taking the solubility as the index， the preparation process parameters of STBLP were optimized by single factor experiment and Box-Behnken response surface method. RESULTS The optimal freeze-drying process for STBLP was obtained： pre-freezing time of 4 h， total drying time of 13 h （before at 0 ℃）， and resolution drying temperature of 25 ℃. The average solubility of 3 batches of STBLP prepared according to the optimal process was 95.72% （RSD＝0.68%， n＝3）， the relative error of which was －0.97% to the theoretical solubility （96.66%）. CONCLUSIONS Optimized lyophilization process in this study are stable and feasible， the solubility of the prepared sample is high.
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OBJECTIVE To establish the method for monitoring the dynamic changes of odor components in Cornus officinalis during processing . METHODS The decoction pieces of C. officinalis with different processing time were prepared by the wine steaming method . The dynamic changes of odor components were obtained by using ultra -fast gas electronic nose ；odor components were identified by comparing with AroChemBase database ；the dynamic changes of odor compounds were analyzed in combination with peak area ，and the chemical pattern recognition analysis were carried out . RESULTS A total of 12 common peaks of odor components were identified in the fingerprints of raw C. officinalis，and 21 in the fingerprints of decoction pieces of C. officinalis. Eight odor components with the high proportion of peak area during processing were ethanol ， isopropyl alcohol ， 2- methylpropylaldehyde，ethyl acetate ，2-methylbutanal，isoamyl alcohol ，2-hexanol and furfural ，among which ，the peak areas of ethanol，isoamyl alcohol and 2-hexanol showed a trend of first increasing and then decreasing ；at 24 h of processing ，their peak areas were still higher than those of raw products . The peak areas of ethyl acetate ，2-methylbutanal and furfural nearly increased with the increase of processing time . Variable importance in projection of above eight odor components were all greater than 1. CONCLUSIONS The method is established for monitoring the dynamic changes of odor components of C. officinalis during processing. Eight odor components such as ethanol can be used as monitoring indicators of C. officinalis dring processing .
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ObjectiveIn order to find a fast odor-based method for the identification of sulfur fumigated Gastrodiae Rhizoma， an ultra-fast gas phase electronic nose technology was used to identify the odors of different degrees of sulfur fumigated Gastrodiae Rhizoma decoction pieces. MethodHeracles NEO ultra-fast gas phase electronic nose was employed to collect gas chromatograms of unsulfured and sulfured with different degrees of Gastrodiae Rhizoma decoction pieces， gas chromatograms were performed under programmed temperature （initial temperature of 40 ℃， 0.2 ℃·s-1 to 60 ℃， and then 4 ℃·s-1 to 250 ℃）， the sample volume was 5 mL， the incubation temperature was 65 ℃ and incubation time was 35 min. Kovats retention index and the AroChemBase database were used for qualitative analysis， and stoichiometric analysis was performed on this basis. Principal component analysis （PCA）， discriminant factor analysis （DFA） and partial least squares-discriminant analysis （PLS-DA） models were established to identify the Gastrodiae Rhizoma decoction pieces with different degrees of sulfur fumigation. ResultAccording to the comparative analysis of AroChemBase database， there were significant differences in the odor characteristics of sulfur fumigated and non-sulfur fumigated Gastrodiae Rhizoma， cyclopentane， acetone and heptane might be the odor components to distinguish the degree of sulfur fumigation in Gastrodiae Rhizoma decoction pieces. The identification index of PCA model was 81， the accumulative discriminant index of the discriminating factors was 92.09% in DFA model， the supervisory model interpretation rate of PLS-DA model was 0.963 and the predictive ability parameter was 0.956， indicating that PCA， DFA and PLS-DA models could well distinguish Gastrodiae Rhizoma decoction pieces with different sulfur fumigation degrees. ConclusionHeracles NEO ultra-fast gas phase electronic nose can be used as a rapid method to identify and distinguish Gastrodiae Rhizoma decoction pieces with different levels of sulfur fumigation. Meanwhile， it can provide a rapid， simple and green method and technology for identification of traditional Chinese medicine decoction pieces by sulfur fumigation.
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OBJECTIVE To establish the fingerprints of dried Houttuynia cordata and its decoction pieces ，conduct chemometrics analysis and determine the contents of 5 flavonoids such as neochlorogenic acid. METHODS High performance liquid chromatography （HPLC）method was adopted. Using quercitrin as reference ，HPLC fingerprints of 10 batches of dried H. cordata and its decoction pieces were drawn. The similarity evaluation was conducted by Similarity Evaluation System of TCM Chromatographic Fingerprint （2012 edition），the common peaks were also confirmed. SIMCA-P 14.1 software was applied for principal component analysis （PCA）and partial least square-discriminant analysis （PLS-DA），and the variable importance in projection（VIP）value more than 1 was considered as a standard to screen the differential components affecting the quality of these two products ；meanwhile，the contents of 5 components such as neochlorogenic acid in both products were determined by the same HPLC method. RESULTS There were 20 common peaks in 10 batches of dried H. cordata and 10 batches of its decoction pieces with the similarity values more than 0.960. A total of 5 common peaks were identified ，which were neochlorogenic acid （peak 1）， chlorogenic acid （peak 3），cryptochlorogenic acid （peak 4），rutin（peak 7）and quercitrin （peak 11）. The results of PCA and PLS-DA showed that dried H. cordata could be distinguished from its decoction pieces obviously ；the common peaks with VIP value greater than 1 were as follows ：peak 7（rutin），peak 20，peak 5，peak 13，peak 2，peak 18，peak 3（chlorogenic acid ）， peak 14，peak 17 and peak 19. The linear range of neochlorogenic acid ，chlorogenic acid ，cryptochlorogenic acid ，rutin and quercitrin were 3.77-60.29 μg/mL（r＝0.999 7），1.40-22.42 μg/mL（r＝0.999 5），3.76-60.22 μg/mL（r＝0.999 9），2.19-35.06 μg/mL （r＝0.999 9）and 25.49-407.88 μg/mL（r＝0.999 7），respectively. RSDs of precision ，stability（24 h）and reproducibility E-mail：20190394@njucm.edu.cn tests were all lower than 3％. The average recoveries of the above components in these two products were 98.72％-101.12％ and 98.86％ -100.63％ with RSDs less than 3％（n＝9）. In dried H. cordata ，the average contents of 5 components were 0.87，0.33，0.59，0.61 and 6.17 mg/g，while the average contents were 0.42，0.11，0.26，0.23 and 3.16 mg/g in its decoction pieces ，respectively. CONCLUSIONS HPLC fingerprint and the method of content determination are stable and feasible ，which could be used for the quality control of dried H. cordata and its decoction pieces. Besides ，rutin and other components may be the differential components which could affect the quality of these two products ；the average contents of the 5 flavonoids such as neochlorogenic acid in dried H. cordata all decrease after processing.
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OBJECTIVE：To analyze and compare th e contents of 6 kinds of monosaccharide in Astragalus membranaceus from different growth years . METHODS ：2-4 years old A. membranaceus from three areas were extracted with water extraction and alcohol precipitation ，Sevage deproteinization to obtain A. membranaceus polysaccharide. The samples were firstly hydrolyzed with trifluoroacetic acid （TFA）and then derivatized by 1-phenyl-3-methyl-5-pyrazolone（PMP）. HPLC analysis was adopted to determine the contents of 6 kinds of monosaccharide as mannose ，rhamnose，galacturonic acid ，glucose，galactose，arabinose. The determination was performed on Symmetry C 18 column with phosphate buffer solution （pH 6.8）-acetonitrile（84∶16，V/V）as mobile phase at the flow rate of 1.0 mL/min. The detection wavelength was 245 nm，and column temperature was 35 ℃. The sample size was 20 µL. RESULTS ：The contents of mannose ，rhamnose，galacturonic acid ，glucose，galactose and arabinose were 0.50-0.94， 0.76-1.60，3.35-7.86，87.33-275.77，1.95-8.96，2.35-14.04 mg/g，respectively. Total contents of monosaccharide from 2，3，4 years old A. membranaceus were 98.26-139.92，173.81-295.71，122.37-182.41 mg/g，respectively. There was significant difference in the contents of glucose between 3 old years A. membranaceus and 2，4 old years A. membranaceus （162.71-275.77 mg/g vs. 87.33-107.70，111.54-167.26 mg/g，P＜0.05）. CONCLUSIONS ：Above 6 monosaccharides are detected in 2，3，4 years old A. membranaceus，among which the content of glucose is the highest. The content of glucose in 3 years old A. membranaceus is higher than that in 2 and 4 years old A. membranaceus .
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AIM To develop an HPLC method for the simultaneous content determination of five constituents in Chairen Capsules (Bupleuri Radix,Ziziphi spinosae Semen,Chuanxiong Rhizoma,etc.).METHODS The analysis of 80％ methanol extract of this drug was performed on a 30 ℃ thermostatic Merck Purospher STAR C1s column (250 mm × 4.6 mm,5 μm),with the mobile phase comprising of acetonitrile-0.1％ formic acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelengths were set at 237,290 and 335 nm.RESULTS Spinosin,ferulic acid,cinnamaldehyde,liquiritin and ammonium glycyrrhizate showed good linear relationships within the ranges of 0.009 26-0.092 6 μg (R2 =0.999 6),0.056 2-0.562 μg (R2 =0.999 8),0.130-1.30 μg (R2 =0.999 8),0.275-2.75 μg (R2 =0.999 5) and 0.568-5.68 μg (R2 =0.999 2),whose average recoveries were 100.73％,100.62％,100.02％,100.41％ and 99.96％ ％ with the RSDs of 2.20％,1.37％,1.52％,1.30％ and 0.80％,respectively.CONCLUSION This simple,accurate and reproducible method can be used for the quality control of Chairen Capsules.
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OBJECTIVE:To establish a method for the simultaneous determination of rutin ,hesperidin ,arctiin ,liquiritin and glycyrrhizinate in Sangxing oral liquid. METHODS:RP-HPLC was performed on the column of Kromasil C18 with mobile phase of acetonitrile-0.1% phosphoric acid solution(gradient elution) at a flow rate of 1.0 mL/min,the detection wavelength was 276, 348 nm ,column temperature was 30 ℃,and the injection volume was 5 μL. RESULTS:The linear range was 1.068-10.68 μg/mL (r=0.9993)for rutin,9.320-93.20 μg/mL(r=0.9992)for hesperidin,46.91-469.1 μg/mL(r=0.9994)for arctiin,0.5110-5.110μg/mL(r=0.9992) for liquiritin;RSDs of precision , stability and reproducibility tests were less than 3%;recoveries were 95.10% -101.90%(RSD=2.1%,n=9),96.75%-101.80%(RSD=1.4%,n=9),95.69%-100.00%(RSD=1.5%,n=9), 98.22%-104.60%(RSD=2.1%,n=9),respectively. CONCLUSIONS:The method is accurate,sensitive and reproducible,and can be used for the simultaneous determination of rutin,hesperidin,arctiin and liquiritin in Sangxing oral liquid.
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OBJECTIVE:To establish the quality standards for Fufang ningshen granule. METHODS:TLC was used for the qualitative identification of Radix angelicae and White paenoy;HPLC was adopted for the contents determination of spinosin and verbascoside:the column was Kromasil C18 with the mobile phase of acetonitrile-0.1% acetic acid(16∶84,V/V)at a flow rate of 1.0 ml/min,detection wavelength was 330 nm,column temerpature was 30 ℃. RESULTS:The TLC spots of R. angelicae and W. pae-noy were clear with good separation,negative control without interference. The linear range was 0.055 44-0.277 2μg for spinosin(r=0.999 4)and 0.055 98-0.279 9 μg for verbascoside(r=0.999 5);RSDs of precision,stability and reproducibility tests were lower than 3.0%;recoveries were 95.62%-100.53%(RSD=1.77%,n=9) and 95.63%-102.57%(RSD=2.74%,n=9). CONCLU-SIONS:The standard can be used for the quality control of Fufang ningshen granule.
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OBJECTIVE:To establish a method for the contents determination of 4 ingredients in Ligustrum lucidum decoration piece by reference extract method. METHODS:HPLC was performed on the column of XBridge C18 with mobile phase of acetoni-trile-0.1% formic acid(gradient elution) at flow rate of 1.0 ml/min,detection wavelength was 254 nm,column temperature was 30℃and volume injection was 10μl. RESULTS:The linear range was 0.037-0.598 mg for neonuezhenide,0.006-0.101 mg for ac-teoside,0.189-3.023 mg for nuezhenide and 0.314-5.027 mg for specnuezhenide(r≥0.999 0);RSDs of precision,reproducibility and stability tests were no more than 3.8%;recoveries were 98.46%-104.83%(RSD=2.43,n=6),95.55%-104.57%(RSD=3.63, n=6),100.09%-104.39%(RSD=1.45,n=6)and 98.84%-104.97%(RSD=2.02,n=6). CONCLUSIONS:The method is simple, good reproducibility,and can be used for the contents determination of 4 ingredients in L. lucidum decoration piece.
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<p><b>OBJECTIVE</b>To establish a HPLC method for determination of 4 components in different varieties of vinegar backed Rhizoma Curcuma.</p><p><b>METHOD</b>The method was established by using an Elite Hypersil ODS2 column (4.6 mm x 250 mm, 5 microm). The mobile phase comprising acetonitrile (A) and water (B) was used to elute the targets in gradient elution mode. Flow rate and detection wavelength were set at 1 mL x min(-1) and 214 nm, respectively. The column temperature was 25 degrees C and the injection volume was 10 microL.</p><p><b>RESULT</b>All calibration curves showed good linearity with r > 0.999 5. Recoveries measured at three concentrations were in the range of 97.27% - 99.27% with RSD < 3%.</p><p><b>CONCLUSION</b>The validated method is simple, reliable, and successfully applied to determine the contents of the selected compounds in vinegar backed Rhizoma Curcuma. The results of the determination showed that contents of the four components in vinegar backed Curcuma wenyujin were relatively high.</p>
Subject(s)
China , Chromatography, High Pressure Liquid , Methods , Curcuma , Chemistry , Drugs, Chinese Herbal , Rhizome , Chemistry , Sesquiterpenes , Sesquiterpenes, GermacraneABSTRACT
Objective To optimize the extraction procedure for Anmai Granules. Methods With the content of Chlorogenic acid and Cinnamylic acid as indexes, orthogonal table L9(34) was used in the experiment of extracting in alcohol to study the effect of technological parameters (the concentration and dosage of alcohol, extraction times, the time of extraction) on the content of Chlorogenic acid and Cinnamylic acid. Results The optimum process is that 70% alcohol is used as extracting solution adding 9 times amount of solution, extracting 2 times, 1.0 hours for each time. Conclusion The extraction process is stable and suitable for industrial production.
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Objective To establish a method for determination of puerarin content in Jingning capsule. Methods The column was Kromasil (250 mm?4. 6 mm, 5 ?m). The mobile phase consisted of methanol- 0.2% water H3PO4 (20/80), with flow rate of 1 mL/min and the UV detective wavelength set at 250 nm. Results Puerarin showed a good linear at the range of 6.268～125.360 ?g/mL (r=0.999 8). The average recovery was 101.42%, with RSD of 1.22%. Conclusion This method is accurate, simple, repeatable and suitable for the determination of puerarin content in Jingning capsule.
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OBJECTIVE:To study the factors influencing the stability of Chlorogenic acid in Marsdenia tenacissima extract.METHODS:The contents of Chlorogenic acid in Marsdenia tenacissima extract in different solvents,different lighting and different time under the heat were determined by HPLC.RESULTS:The Chlorogenic acid in Marsdenia tenacissima extract in organic solvents was more stable,in addition,lighting and heating temperature were important factors affecting the stability of the Chlorogenic acid.CONCLUSION:The stability of the Chlorogenic acid in Marsdenia tenacissima extract changes in different conditions;and the study results serve as a reference for the preparation,storage,analysis and production of Marsdenia tenacissima extract.
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The optimum conditions for the processing of Sparganium stoloniferum Buch-Ham. withvinegar were studied by L9(3)4 orthogonal experimental design, as guided by decrease of writhing rate inanalgesic test and anticoagulant activity. The results showed that the best processing conditions were stirfrying of the raw S. stoloniferum with the addition of 25 kg of vinegar per 100 kg of crude drug at 130℃for 10 min.
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Objective To establish the fingerprint for the dry stem in Dendrobium candidum by RP-HPLC.Methods Kromasil○RKR100-5 C18 column(250 mm?4.6 mm,5 ?m) was used with a mixture of acetonitrile-0.4% phosphorus acid as mobile phase in a gradient mode and the data were analyzed with ″Computer Aided Similarity Evaluation″ software.Results The chemical constituents of D.candidum were optimally separated,among which 15 fingerprint peaks in common were confirmed.Conclusion This method is simple,accurate with good reproducibility,and can be used specifically for the quality control of D.candidum.
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Objective To study pharmacokinetics of curcumin in Curcuma phaeocaulis in rats in vivo.Methods HPLC method was used to determine the curcumin in rat plasma.The conditions were column: Lichrospher-5-C_(18)(250 mm?4.6 mm, 5 ?m); column temperature: 25 ℃;mobile phase: CH_3CN-5% HAc water solution(45∶55);flow: 1 mL/min;detection wavelength: 420 nm.Results The calibration curve was liner(r=0.999 5) at the range of 6.5—104 ?g/mL.The average recovery was 98.5%.RSD was 2.41%(n=5).The pharmacokinetic parameters of curcumin were as follows: k_a was 0.53/h,k_e was 0.10/h,t_(1/2ka) was 1.32 h,t_(1/2k) was 6.89 h,t_(peak) was 3.89 h,C_(max) was 93.15 ng/mL,AUC was(1 369.38) ng/mL.Conclusion This method is stable,simple,and reliable,which can be applied for the determination of curcumin in plasma and pharmacokinetic studies.
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Objective To establish the chromatography fingerprint of Radix Scrophulariae by RP-HPLC.Methods HPLC was applied in this study.Kromasil KR100-5C18(4.6 mm? 250 mm,5 ? m)column and DAD detector were used with a mixture of methanol and 0.1 % methanoic acid as mobile phase in a gradient mode.Results The chemical substances of Radix Scrophulariae were optimally separated.Conclusion This method is simple,accurate with good reproducibility,thereby can be used specifically for the quality control of Radix Scrophulariae.
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AIM: To establish a method for determining total flavonoids in Compound Ginkgo Granules so as to control the quality. METHODS: HPLC conditions: YWG-C_ 18 column, mobile phase: V(MeOH)∶V(1%HAC)=50∶50, flow rate: 1.0 mL/min, detection:?=360 nm, column temperature: 25 ℃. RESULTS: The calibration curve of quercetin、 kaempferol and isorhamnetin was linear in range of 0.057 2 -0.286 0 ?g, 0.074 0 -0.370 0 ?g, 0.029 4 -0.147 0 ?g, respectively. The average recovery was 98.39% , and RSD was 1.25 (n=6). CONCLUSION: This method is rapid, accurate and reproducible and could be used for quality control of Compound Ginkgo Granules.
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AIM: To study the blood quickening and stasis dispelling effect of the different processed products of Rhizoma Curcumae by rat's platelet aggregation in vivo and its hemorrheological properties and blood coagulation. METHODS: The platelet aggregation determination, hemorrheological properties determination and mice blood coagulation method were used to observe the blood quickening and stasis dispelling effect of the different processed products of Rhizoma Curcumae. RESULTS: The different processed products of Rhizoma Curcumae all had some inhibition on platelet aggregation, anticoagulation and improvement on the hemorrheological parameters. Among all of them, the processed product with vinegar was the most strong. CONCLUSION: In traditional processes, pharmacological test shows that Rhizoma Curcumae processed with vinegar has the best effects.
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AIM: To research the best processing method of Rhizoma Curcumae with water.METHODS: L 9(3 4) orthogonal table are decided with three effects: moistening time, steaming time, thickness of processed pieces. According to the amount of curcumin and volatile oil, orthogonal Design is applied to water processing Rhizoma Curcumae.RESULTS: The best processing method is: Rhizoma Curcumae is moistened for 20min, then cutting up to 3mm thick after steaming 30min.CONCLUSIONS:The steaming time has no obvious effect on the amount of curcumin in Rhizoma Curcumae, but if the amount of volatile oil is taken as marker. the steaming time has obvious effect.