Study on odor composition change of traditional Chinese medicine sachet during placement based on ultra-fast gasphase electronic nose technology / 中国药房

OBJECTIVE To analyze the odor composition changes of two kinds of traditional Chinese medicine sachet （children type and adults type） with different placement time by using ultra-fast gasphase electronic nose technology. METHODS The change rule of sachet components at different storage times was analyzed by gas chromatography. At the same time， the qualitative results were obtained by combining electronic nose with Arochembase database. Discriminant factor analysis was used to analyze the overall odor composition differences of the two sachet samples. RESULTS A total of 10 odor compositions were identified in children-type sachet， including α-pinene and β-pinene as the functional index compositions； five odor compositions of children-type sachet disappeared after 0.25 days， and most of them disappeared after 7 days； the cumulative contribution rate of discriminant factor analysis was 99.225%. A total of 8 odor compositions were identified in adult-type sachets， including α-pinene and α-phellandrene as the functional index compositions； four odor components disappeared after the adult-type sachet was placed for 0.25 days； after 15 days of placement， the peak 6-8 disappeared， and the intensity of peak 5 decreased by 34.3% compared with 0 day of placement； the cumulative contribution rate of discriminant factor analysis was 91.965%. CONCLUSIONS With the extension of storage time， the smell and composition of the two traditional Chinese medicine sachets are decreasing. It is recommended that the use time of children-type sachet is 7 days， and that of adult-type sachet is 15 days.

Optimization of the preparation process of Soft-shelled turtle blood lyophilized powder using Box-Behnken response surface methodology / 中国药房

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.

Rapid Identification of Gastrodiae Rhizoma with Different Sulfur Fumigation Levels Based on Ultra-fast Gas Phase Electronic Nose / 中国实验方剂学杂志

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.

Study on dynamic changes of odor components in Cornus officinalis during processing by ultra -fast gas phase electronic nose / 中国药房

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 .

Study on the fingerprint establishment ，chemometrics analysis and content determination of dried Houttuynia cordata and its decoction pieces / 中国药房

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.

Identification of the Origin of Schizonepeta tenusfolia Based on “Odor”Information / 中国药房

OBJECTIVE：To esta blish the m ethod for identifying Schizonepeta tenusfolia from different habitats based on odor information. METHODS ：The odor of S. tenusfolia from different habitats were identified by Heracles Ⅱ ultra-fast gas phase electronic nose. Qualitative analysis was conducted according to obtained chromatographic information combined with AroChemBase database and Kovats retention index qualitative database. Principle component analysis （PCA）and discriminant factor analysis （DFA）were conducted by using Alpha Soft V 14.2 software，and cluster analysis （CA）was performed with SPSS 22.2 software. RESULTS ：There were 16 common peaks in 15 batches of S. tenusfolia from different habitats. After comparison with AroChemBase database and Kovates retention index qualitative database ，a total of 13 possible components were obtained. The possible components and sensory description information of S. tenusfolia from different habitats were basically the same ，but only the content was different. The chromatographic peak intensities of common peak No. 2 were in descending order as Anhui ＞ Gansu＞Henan＞Hebei＞Jiangsu，the chromatographic peak intensities of common peak No. 6 were in descending order as Anhui ＞ Hebei＞Gansu≈Henan＞Jiangsu，the chromatographic peak intensities of common peak No. 9 were in descending order as Anhui ＞ Gansu＞Henan＞Jiangsu＞Hebei，the chromatographic peak intensity of common peak No. 13 were in descending order as Anhui ≈ Gansu＞Hebei＞Jiangsu＞Henan，which represented the chromatographic peak intensity of methyl formate （peak No. 2），α-pinene （peak No. 6），3-nonone（peak No. 9）and α-terpineol（peak No. 13）were significantly different due to the change of habitats. PCA results showed that the cumulative contribution rate of the first two principal components was 96.807％. Results of DFA showed that contribution rates of discriminant factor 1 and discriminant factor 2 were 92.089％ and 3.982％. CA results showed that when the distance was 10，15 batches of samples could be clustered into 3 categories，B1-B5 and J 1-J3 into one category ，A1-A3 into one category ，G1，G2，N1 and N 2 into one category. The results were basically consistent with those of PCA and DFA. CONCLUSIONS：Ultra-fast gas phase electronic nose technology can be used to identify S. tenusfolia from different habitats rapidly. Methyl formate ，α-pinene，3-nonone and α-terpineol may be the key factors to distinguish S. tenusfolia from different habitats.

Simultaneous determination of five constituents in Chairen Capsules by HPLC / 中成药

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.

Simultaneous Determination of Rutin, Hesperidin,Arctiin and Liquiritin in Sangxing Oral Liquid by RP-HPLC / 中国药房

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.

Study on the Quality Standard for Fufang Ningshen Granule / 中国药房

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.

Optimal dose of Ligustrazine nanoparticles in a rat model of experimental peritoneal adhesion / 中国组织工程研究

BACKGROUND:Ligustrazine can effectively prevent and treat peritoneal adhesion and adhesive ileus after surgical treatment. OBJECTIVE:To prepare Ligustrazine nanoparticle spray which is prepared to achieve sustained release and improve clinical efficacy and to explore its optimal dose for preventing experimental peritoneal adhesions in rats. METHODS:Eighty rats were randomly divided into five groups:model group, sodium hyaluronate group, high-, medium-and low-dose Ligustrazine nanoparticle groups, with 16 rats in each group. After peritoneal adhesion model was established with rasp method, model group was immediately subject to abdomen-closing, while sodium hyaluronate group and Ligustrazine nanoparticle groups received sodium hyaluronate smearing and Ligustrazine nanoparticle spray (2.5, 5, 10 mg/kg), respectively. Al rats were kil ed at 1 and 2 weeks after modeling, to observe adhesions. The adhesion score was recorded. The adhesive tissue sections were stained with hematoxylin-eosin for pathological changes. The level of transformation growth factor-β1 in peritoneal fluid of rats was detected with ELISA assay. RESULTS AND CONCLUSION:Ligustrazine Nanoparticle spray had a sustained release effect, and prolonged the duration of action of drugs, thus achieving a better anti-adhesion effect post-surgery. The medium-and high-dose Ligustrazine nanoparticle sprays exhibited better anti-adhesion effects, and improved the rise of transformation growth factor-β1 level in the peritoneal fluid. As the drug concentration is low, the intraperitoneal administration in a spray manner is preferred. Because the total dose is limited, we define the optimal effective dose as 5 mg/kg.

Comparison of content of curdione, curcumol, germacrone and beta-elemene in different varieties of vinegar backed Rhizoma Curcuma / 中国中药杂志

<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>

Optimization of the Extraction Technology for Gengniankang Granules with the Multiple Guidelines Grading Method / 中国中医药信息杂志

Objective To optimize the extraction technology for Gengniankang Granules.Methods An orthogonal test was adopted in the study.The contents of Paeoniflorin and Astragaloside Ⅳ were used as indices of appraisal.Data processing was carried out with the multiple guidelines grading method for optimizing the extraction condition.Results The optimized extraction technology for Gengniankang Granules was shown to be:eighteen fold volume of 70% alcohol should be added to 1 volume of the granules for 3 successive reflux extractions with 1.5 h of each.Conclusion The optimized extraction technology was rational and the extraction rate of the active components was high.

Stability of Chlorogenic Acid in Marsdenia Tenacissima Extract / 中国药房

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.

Optimization of Processing Technique of Sparganium stoloniferum by Orthogonal Experimental Design / 中草药

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.

Pharmacokinetic studies on curcumin in Curcuma phaeocaulis in rats in vivo / 中草药

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.

Study on the Chromatography Fingerprint of Radix Scrophulariae by RP-HPLC / 中药新药与临床药理

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.

Study on quality standard of Huganbadu Ointment / 中成药

Objective: To develop the quality standard of Huganbadu Ointment(Radix Sophorae Flavescentis, Herba Artemisiae Annuae, Radix Astragali, Radix Paeoniae Rubra, etc.) Methods: Radix Sophorae Flavescentis, Herba Artemisiae Annuae, Radix Astragali and Radix Paeoniae Rubra were identified by TLC and the content of matrine was determined by TLC Scanning. Results: The identification study showed strong specificity. The average recovery of matrine was 97.11%, and RSD was 2.50%. Conclusion: The methods established can be used for the quality control of the preparation.

Study on preparation of ?-cyclodextrin inclusion compound of volatile oil from Curcuma wenyujin / 中成药

Objective:To study optimum inclusion process conditions for volatile oil from Curcuma wenyujin. Methods: The study was carried out with orthogonal design. The process conditions were studied by determining the ultizision ratio of volatile oil from Curcuma wenyujin , the oil bearing rate and extract ratio of inclusion compound. Results: The optimum preparation conditions for inclusion were established as∶oil∶? CD was 1∶9, The inclusion temperature and time were at 40 ?C and for 1.5h , The ultizision ratio of oil was 86.5% . Conclusions: The rate is high and the method is applicable.

Determination of quercetin, kaempferol,isorhamnetin and flavonoids in Compound Ginkgo Granules by HPLC / 中成药

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.