Exploration on Determination and Quantity Transfer of Index Components in Benchmark Samples of Erdongtang / 中国实验方剂学杂志

ObjectiveTo establish the determination for index components in benchmark samples of Erdongtang， and clarify the content and transfer rate rages of index components in 15 batches of benchmark samples， and to explore the quantity transfer of index components of decoction pieces to benchmark samples. MethodFifteen batches of benchmark samples were prepared， the contents of mangiferin， baicalin and glycyrrhizic acid were determined by high performance liquid chromatography （HPLC）-diode array detector （DAD）， the mobile phase was acetonitrile （A）-0.1% formic acid aqueous solution （B） for gradient elution （0-10 min， 10%-17%A； 10-25 min， 17%-19%A； 25-28 min， 19%-25%A； 28-45 min， 25%-33%A； 45-46 min， 33%-45%A； 46-60 min， 45%-55%A）， detection wavelength was set at 254 nm. Contents of timosaponin BⅡ and the sum of protoneodioscin and protodioscin were determined by HPLC-evaporative light scattering detector （ELSD）， the mobile phase was acetonitrile （A）-water （B） for gradient elution （0-20 min， 24%A； 20-25 min， 24%-27%A； 25-33 min， 27%-28%A； 33-36 min， 28%-90%A； 36-41 min， 90%-24%A）. ResultThe methodological verification of the established method was good， which could be used for determination of five index components in benchmark samples. The content ranges of mangiferin， baicalin， glycyrrhizic acid， timosaponin BⅡ， and the sum of protoneodioscin and protodioscin in 15 batches of benchmark samples of Erdongtang were 0.14%-0.23%， 2.40%-3.37%， 0.07%-0.44%， 0.43%-0.95%， and 0.15%-0.47%， the transfer rate ranges of them were 33.90%-52.15%， 84.46%-105.61%， 22.59%-93.86%， 38.07%-61.43%， and 53.28%-96.11%， respectively. ConclusionThe consistencies of transfer rate of mangiferin， baicalin， timosaponin BⅡ and the sum of protoneodioscin and protodioscin （except glycyrrhizic acid） between decoction pieces and benchmark samples of Erdongtang are good， indicates that the transfer rates of 4 index components are stable during the preparation process of benchmark samples， which can provide data support for research and development of the compound preparation of this formula.

Increases in alginate production and transcription levels of alginate lyase (alyA1) by control of the oxygen transfer rate in Azotobacter vinelandii cultures under diazotrophic conditions

BACKGROUND: Alginates are polysaccharides used in a wide range of industrial applications, with their functional properties depending on their molecular weight. In this study, alginate production and the expression of genes involved in polymerization and depolymerization in batch cultures of Azotobacter vinelandii were evaluated under controlled and noncontrolled oxygen transfer rate (OTR) conditions. RESULTS: Using an oxygen transfer rate (OTR) control system, a constant OTR (20.3 ± 1.3 mmol L 1 h 1 ) was maintained during cell growth and stationary phases. In cultures subjected to a controlled OTR, alginate concentrations were higher (5.5 ± 0.2 g L 1 ) than in cultures under noncontrolled OTR. The molecular weight of alginate decreased from 475 to 325 kDa at the beginning of the growth phase and remained constant until the end of the cultivation period. The expression level of alyA1, which encodes an alginate lyase, was more affected by OTR control than those of other genes involved in alginate biosynthesis. The decrease in alginate molecular weight can be explained by a higher relative expression level of alyA1 under the controlled OTR condition. CONCLUSIONS: This report describes the first time that alginate production and alginate lyase (alyA1) expression levels have been evaluated in A. vinelandii cultures subjected to a controlled OTR. The results show that automatic control of OTR may be a suitable strategy for improving alginate production while maintaining a constant molecular weight.

Determination of three saponins in Compound Shiwei Tablets and study on transfer rate in its preparation process / 中草药

Objective: High performance liquid chromatography-evaporative light scattering detector (HPLC-ELSD) method was used to establish the determination method for the three kinds of saponins (astragaloside I, II, and IV) in Compound Shiwei Tablets (CST), and investigate the three saponins components’ s transfer rate in the preparation process of CST in order to improve the quality control method of CST. Methods: A HPLC-ELSD method was operated on the column of Agilent 5-HC C18 (2) (250 mm × 4.6 mm, 5 μm), with acetonitrile-water as the mobile phase for gradient elution, at a flow rate of 1.0 mL/min, with column temperature of 30 ℃ and injection volume of 20 μL. The ELSD parameters were as follow: the carrier gas flow rate was 1.5 L/min, the drift tube temperature was 90 ℃. Determinate the content of astragaloside I, II, and IV in products, granules and extracts of CST, and calculate the transfer rate of three saponins in the preparation process of CST. Results: A method for the determination of astragaloside I, II, and IV in CST was established. Under this condition, all three components reached baseline separation with good linear relationship. The average recovery rates were 99.58%, 99.31% and 99.51%, and RSD values were 3.0%, 2.5% and 2.5%, respectively. Astragaloside I had lower transfer rate during the preparation process, and the transfer rate of astragaloside IV was the higher in the preparation process, both of which were greater than 100%. Conclusion: This study established a method for simultaneous determination of three kinds of saponins of astragaloside I, II, and IV in CST. The method has good reproducibility and strong specificity, which is simple and easy,and can be used to inspect the transfer rates of three kinds of saponins in the preparation process and improve the quality control standard of saponins in CST, and provide reference for the quality control of other traditional Chinese medicine preparations containing astragalus.

Preparation and process quality control of substance benchmarks of classical famous prescription of Baihe Dihuang Decoction / 中草药

Objective: To prepare substance benchmarks of Baihe Dihuang Decoction (BDD), and evaluate the scientificity and rationality of preparation process by analyzing the process quality. Methods: Fifteen batches of substance benchmarks were prepared according to the ancient method, the content of catalpol and acteoside in the preparation process was determined, and the transfer rate and extractum rate were calculated. Fingerprints of 15 batches of decoction pieces, decoction, concentrate and substance benchmarks were detected by HPLC, and the common peaks of fingerprints were attributed and identified; In addition, the similarity of fingerprints were evaluated. Results: In 15 batches of substance benchmarks, the transfer rates of catalpol and acteoside were 81.40%—92.88% and 28.90%—41.41% respectively, the extractum rate was 36.06%—41.71%, and without discrete data. During the process of decoction, concentration and freeze-drying, the transfer rates of effective components were stable. In the fingerprints of substance benchmarks, 16 common peaks were determined, of which six peaks belong to Lilii Bulbus, nine peaks belong to Rehmanniae Radix. Three peaks were identified. The similarity of fingerprints of decoction pieces, decoction, concentrate, and substance benchmarks were all over 0.9. The similarity of reference fingerprints of decoction, concentrate, and substance benchmarks were over 0.99. Conclusion: The fingerprint method is reasonable and feasible, which can be used for simultaneously determining the fingerprint of decoction pieces, intermediates and substance benchmarks. The preparation process is scientific and reasonable, and will not changes substance basis significantly. The paper establishes a foundation for the development of preparation of BDD, and provides a new idea for the evaluation of process and quality of the substance benchmarks of classical famous prescriptions.

Quality Evaluation of Standard Decoction of Zingiberis Rhizoma / 中国实验方剂学杂志

Objective: To establish the quality control methods for the standard decoction of Zingiberis Rhizoma. Method: DNA barcode primitives were identified for the medicinal materials from different origins; according to the standard of Chinese herbal medicine decoction preparation principle,the identified Zingiberis Rhizoma was prepared into standard decoction for analysis. Meanwhile, the extraction method and analysis method were validated from methodologies, and the transfer rate of 6-gingerol as well as the extraction rate of standard decoction of Zingiberis Rhizoma were calculated. In addition,the quality standard of standard decoction of Zingiberis Rhizoma was also established based. The structures of main chromatographic peaks were identified by ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) to clarify the main chemical constituents in the standard decoction of Zingiberis Rhizoma. Result: All the samples were identified as Zingiberis Rhizoma. Under the conditions established in this paper,the standard curve of 6-gingerol was Y=661.56X+2.493 3(r=0.999 3),and the RSD was 0.5%in precision test, indicating that the instrument precision was good. The repeatability test showed that the RSD was 0.3%, indicating that the method had good repeatability. The stability test showed that the RSD was 0.4%, indicating that the test solution had good stability within 24 h. The recovery rate was 97.2%and the RSD was 0.6%,indicating that the method was accurate and reliable. 6-gingerol's transfer rate ranged from 31.8%to 57.4%and the extraction rate was within the range of 9.6%-23.1%. The fingerprint similarity of 12 batches of Zingiberis Rhizoma standard decoction was>90%. Conclusion: The established quality control method for Zingiberis Rhizoma was stable and feasible; meanwhile, the standard preparation method for Zingiberis Rhizoma and its quality evaluation system were also established in this study.

Quality Evaluation System of Standard Decoction of Puerariae Thomsonii Radix / 中国实验方剂学杂志

Objective: To establish the quality control methods for the standard decoction of Puerariae Thomsonii Radix.Method:According to the preparation principles for traditional Chinese medicine (TCM) standard decoction,13 batches of Puerariae Thomsonii Radix from different origins were analyzed under the chromatography conditions established in this study and verified with methodology.By referring to Chinese Pharmacopoeia of 2015,puerarin was used as a quantitative indicator to calculate the transfer rate.In this study,the structures of main chromatographic peaks were also identified to clarify the main chemical constituents in the standard decoction.Result:The 13 batches of medicinal herbs were identified as Puerariae Thomsonii Radix,with a recovery rate of 98.0%,and RSD of 1.1%,indicating that the method was accurate and reliable.The transfer rate ranged from 41.4% to 60.0%,and the extraction rate was within the range of 15.7%-34.3%.The corresponding fingerprints were prepared for 13 batches of the standard decoction,and their similarities were all greater than 90.0%.The chemical constituents from Puerariae Thomsonii Radix were identified by mass spectrometry analysis,including citric acid,4'-O-glucosyl puerarin/daidzein-4',7-diglucoside,3'-hydroxy puerarin/genistein puerarin,puerarin apioside,daidzin puerossid A and daidzein,etc.Conclusion: The 13 batches of Puerariae Thomsonii Radix decoction in different origins had consistent properties with the basic properties of medicinal decoction pieces.The established method of quality evaluation can be used to systematically evaluate the standard decoction,providing reference for quality control of related decoction preparations of Puerariae Thomsonii Radix.

Study on Quality Standard of Fried Perilla frutescens Seed Standard Decoction / 中国药房

OBJECTIVE： To prepare standard decoction of fried Perilla frutescens seed and study the quality standard. METHODS： According to the preparation requirements of standard decoction， 17 batches of standard decoction of fried P. frutescens seed were prepared， and the yield of paste was calculated. HPLC method was used for quantitative analysis of rosmarinic acid in standard decoction of fried P. frutescens seed. The determination was performed on Agilent 5 TC-C18（2） column with mobile phase consisted of methanol-0.1％ formic acid solution （40 ∶ 60， V/V） at the flow rate of 1.0 mL/min. The detection wavelength was set at 330 nm， and column temperature was 30 ℃. The sample size was 5 μL. The transfer rate was calculated. HPLC fingerprint was established for 17 batches of standard decoction of fried P. frutescens seed， and analyzed by using TCM Chromatogram Fingerprint Similarity Evaluation System （2012 edition）. The chromatogram peaks were identified by comparing retention time of common peak. RESULTS： The yield of paste were 5.55％-9.75％ in 17 batches of standard decoction of fried P. frutescens seed. The contents of rosmarinic acid were 0.44％-1.58％， and average content was 1.08％. The transfer rates of rosmarinic acid were 18.31％-34.32％， and average transfer rate was 25.42％. In HPLC fingerprints for 17 batches of standard decoction of P. frutescens seed， a total of 11 common peaks were identified， and the similarity was higher than 0.95. Five common peaks were identified， namely caffeic acid （peak 3），luteolin （peak 5）， rosmarinic acid （peak 8） ， luteolin （peak 9）， apigenin （peak 10）. CONCLUSIONS： The quality control method of standard decoction of fried P. frutescens seed is established， which can provide reference for the formulation of the quality standard of fried P. frutescens seed granules and related preparations.

Explore correlation between quality of standard decoction and marker component amygdalin of decoction slices of blazing Armeniacae Semen Amarum / 中草药

Objective To explore the relevance between the quality of standard decoction and the marker component amygdalin of decoction slices of blazing Armeniacae Semen Amarum (BASA) by mathematical model. Methods The BASA standard decoction was prepared, and three linear regression models of the amygdalin content and dry extract rate, the content of amygdalin in standard decoction and decoction slices, and the transfer rate in standard decoction and the content of amygdalin in decoction slices were established by using Design-Expert 8.0.6 software, respectively. Results The dry extract rate of BASA was 8.97%-12.12%; The content of amygdalin in standard decoction was 21.74%-30.32%; And the transfer rate of amygdalin was 70.39%-90.54%. The R2 values of three linear regression models were all greater than 0.8. The P values of each partial regression coefficient were less than 0.05, which indicated that the three models were significant. Then the accuracy of three linear regression models was verified. The relative deviation between the predicted and measured values was less than 10%, and the average relative deviation was not greater than 5%. Conclusion The models established in this study could predict the quality of standard decoction prepared from different BASA, and provide a certain reference value for the establishment of standard decoction quality standard.

Study of Transfer Rate of Standard Decoction of Dipsacus asper Decoction Pieces / 中国药房

OBJECTIVE:To study transfer rate of asperosaponinⅥ in standard decoction of Dipsacus asper decoction pieces. METHODS:The content of asperosaponin Ⅵ in Dipsacus asper decoction pieces and its standard decoction was determined by HPLC. The determination was performed on SinoChrom ODS-AP with mobile phase consisted of acetonitrile-water(30∶70,V/V)at the flow rate of 1.0 mL/min. The detection wavelength was set at 212 nm,and column temperature was 30℃. The sample size was 10 μL. By the ingredients content obtained,the transfer rate of asperosaponin Ⅵ was calculated during decoction piece to standard decoction. RESULTS:The linear range of asperosaponin Ⅵ was 0.484-4.84 μ g(r＝0.999 9). RSDs of precision,stability and reproducibility tests were all lower than 2%. The limits of quantification and detection were 0.3 and 0.1 μ g,respectively. The average recoveries in D. asper decoction pieces and standard decoction were 95.13% -100.22%(RSD＝1.78%,n＝6), 97.07%-100.08%(RSD＝0.98%,n＝6). RSD of durability test was lower than 1%.The transfer rate of asperosaponin Ⅵ in standard decoction of D. asper decoction pieces ranged 26.3%-49.5%. CONCLUSIONS:The method is simple,accurate,precise, stable,reproducible and durable,and can be used for transfer rate of asperosaponin Ⅵ in standard decoction of D. asper decoction pieces.

N1 characteristics and influencing factors in non-small cell lung cancer of T2 stage / 中国胸心血管外科临床杂志

@#Objective    To investigate the characteristics and influencing factors of N1 in T2 stage of the 8th TNM stage of The International Association for the Study of Lung Cancer (IASLC) (3 cm <tumor size≤5 cm) non-small cell lung cancer (NSCLC), to provide the basis for dissecting intrapulmonary lymph node more accurately during the operation. Methods    We collected the clinical information of patients who underwent the pulmonary malignant tumor surgery in Dalian Central Hospital between October 2011 and November 2016. Through the inclusion and exclusion criteria, a total of 68 patients were obtained, including 48 males and 20 females, aged 48–81 (63.1±7.6) years. According to the pathological results, we invesigated the characteristics and influencing factors of N1 in T2 stage non-small cell lung cancer. Results    The results showed that the highest positive rate of lymph node was 14.8% in the 12th group, 14.3% in the 13th group, and 13.9% in the 6th group, respectively. In the single factor analysis, it showed that male, T2b stage, poorly differentiated degree were the risk factors for intrapulmonary lymph node metastasis in T2 stage (P<0.05). But the intrapulmonary lymph nodes metastasis was no significant correlation with above factors according to the multivariate analysis. Conclusion    It is necessary to extract the intrapulmonary lymph node of T2 stage NSCLC at utmost, especially for the No.12 and No.13 high-risk areas. T2b stage with odd ratio (OR) at 3.038 and poorly differentiated degree (OR=1.945) may be the risk factors for the intrapulmonary lymph nodes metastasis of NSCLC in T2 stage. But they are not determining factors.

Quality evaluation of Rhei Radix et Rhizoma decoction / 中国中药杂志

Decoction of single medicinal herb is a reference for the standardization of different dosage forms of Chinese medicine and it provides a new direction for solving the problems existing in the quality of Chinese medicinal granules such as no uniform dosage form and no clear quality standard. In this paper, the quality evaluation method of standard decoction of rhubarb was established to provide reference for the quality control of common dosage forms such as clinical decoction and formula granule. 10 batches of representative Rhei Radix et Rhizoma were collected to establish UPLC fingerprints were established. The chemical structures of main peaks were identified with ultra-performance liquid chromatography with quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS) and the main components in the decoction were Anthraquinones. The extraction ratio of the standard decoction was (28.1±3.8)% and the transfer rate was (19.9±6.3)%. The method for the quality evaluation of standard decoction of Rhei Radix et Rhizoma was established in this study, providing reference for the quality control method of terminal products from decoction of Rhei Radix et Rhizoma.

Quality evaluation of medicinal herb decoction--Forsythiae Fructus / 中国中药杂志

To establish the quality control methods for the standard decoction of Forsythiae Fructus. Twelve batches of representative Forsythiae Fructus were collected to prepare standard decoction of Forsythiae Fructus, and then the parameters such as extraction ratio, transfer rate of the index components and pH value of the solution were calculated to evaluate the stability of the process. The simultaneous determination method of target components and fingerprint method were established, and ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) was used to identify the main common peaks in the fingerprint to clarify the main chemical constituents in the decoction. The similarities of the fingerprints of standard decoction of Forsythiae Fructus were more than 0.9. The average extraction ratio of the standard decoction of Forsythiae Fructus was (15.53±6.27)%, and the transfer rate of forsythiaside A was(38.0±10.2)%. The method for evaluating the quality of standard decoction of Forsythiae Fructus was presented, providing reference for the quality control of products stemmed from the water extract of Forsythiae Fructus, with high similarity and uniform quality.

Optimization of Dry Granulation Technology for Yinqiao Baidu Tablet by Orthogonal Test / 中国药房

OBJECTIVE:To optimize the dry granulation technology conditions for Yinqiao baidu tablet. METHODS:Using granulating difficulty degree and disintegration time as investigation indexes,ratio and amount of accessories microcrystalline cellu-lose and compressible starch in Yinqiao baidu tablet,moisture content of the sprayed powder were screened. Using yield of particle and angle of repose as indexes,L9(34)orthogonal test was used to optimize the wheel pressure,rotating speed and feeding speed in dry granulation technology,and verification test was conducted. RESULTS:The ratio of microcrystalline cellulose and compress-ible starch was 7:3,and mixing ratio of the two with spray powder+inclusion compound was 1:5. The moisture content of spray powder was controlled in 1％-2％. The optimal technology was as follow as wheel pressure of 3.5 MPa,roller speed of 4 r/min and feeding speed of 10 r/min. In verification test,average yield of particle was 69.2％ and angle of repose was 31.5 °. Transfer rate of chlorogenic acid had reached over 92％,and RSD of each index was below 2.53％(n=3). CONCLUSIONS:Each index of parti-cle prepared by optimized accessories formulation and technology shows good reproducibility and feasibility,and the technology is stable and suitable for production.

Enriching technic-process of juglone-constituents from Qinglongyi / 国际药学研究杂志

Objective To optimize the best macroporous resin through static adsorption and desorption and establish enrichment process of juglone-constituents from Qinglongyi with the transfer rate of juglone constituents as the index. Methods The static adsorption and desorption of four different resins with different polarity to juglone-constituents from Qinglongyi were compared. AB8 resin was selected as the best resin. Results The craft parameters of the best resin were optimized, and the results were as follows: initial concentration was 0.0760 g/ml, the pH was 2.0, the flow rate of adsorption was 3BV/h, the elution concentration of ethanol was 70%, the elution volume was 3BV,the desorption flow rate was 2BV/h, and the ratio of diameter to height was 1:10. After the process of optimization, the content of juglone- constituents from Qinglongyi increased from 1.026% to 11.08% and the transfer rate was 72.08%. Conclusion The AB8 macroporous resin could be used to enrich and purify juglone-constituents from the Qinglongyi.

Quality evaluation of decoction of single medicinal herb--a case of Lonicerae Japinicae Flos / 中国中药杂志

Decoction of single medicinal herb is a reference for the standardization of different dosage form of Chinese medicine and it provides a new direction for solving the problems existing in the quality of Chinese medicinal granules such no uniform dosage forms and no clear quality standard. There are few reports on the idea, method and preparation of single herb standard decoction. Our country is in urgent need of that information in order to improve the consistency and stability of traditional Chinese medicine products. Here, Lonicerae Japinicae Flos was selected as an example to elucidate the preparation and quality evaluation of Chinese single herbal medicine decoction. Twelve batches of representative Lonicerae Japinicae Flos were collected, UPLC fingerprints were established, and the chemical structures of main peaks were identified with UPLC-QTOF-MS and standard compounds. The main components in the decoction are organic acids and iridoids. The extract rate of the standard decoction was (34.2±2.9)% and the transfer rate is (78.6±8.4)% in the form of chlorogenic acid, within the range of 75%-125% of mean. This paper established a method for the quality evaluation of standard decoction of Lonicerae Japinicae Flos and provided reference for the quality control method of terminal products from decoction of Lonicerae Japinicae Flos.

Establish quality evaluation method based on standard decoction of Danshen extract / 中国中药杂志

The quality of Danshen extract granules on market is largely different from each other mainly due to the heterogeneous quality of raw materials of Salvia miltiorrhiza, various producing procedures and lack of good quality evaluation method. Formula granule and "standard decoction" have the same quality. In this paper, a systematic evaluation method for the quality of Danshen decoction was established from the perspective of "standard decoction", in order to explore the main factors affecting the quality uniformity of Danshen extract granules. Danshen standard decoction was prepared; then the fingerprint method was developed to determine the content of salvianolic acid B; and the main peaks in the fingerprint were identified with UPLC-QTOF/MS to clarify the chemical compositions of Danshen decoction. Three indexes were calculated to evaluate the stability of whole process, including the extraction ratio; transfer rate of index components and pH value. The results showed that the main components of Danshen decoction were phenolic acids, while the extraction rate, the transfer rate of salvianolic acid B and pH value were in a relatively stable level, and the similarity in the fingerprint of standard decoction was high, indicating that the preparation procedure was stable. The level of salvianolic acid B in the standard decoction was in a large range, which was mainly due to the difference in the quality of Salviae Miltiorrhizae Radix et Rhizoma.

Establish quality evaluation system for standard Ephedrae Herba decoction / 中国中药杂志

To establish the quality control methods for the standard decoction of Ephedrae Herba, and provide the reference for quality evaluation method of all Chinese herbal medicine decoction.Standard decoction of Ephedrae Herba was prepared, and UPLC-UV fingerprint was established to determine the total contents of ephedrine and pseudoephedrine. Then UPLC-QTOF/MS was used to confirm the major common peaks in the fingerprint to clarify the main chemical constituents in the decoction. In addition, the stability of the process was evaluated by calculating the parameters such as the extraction ratio, transfer rate of the index components and the pH values.In the decoction of Ephedrae Herba, the total average concentration of ephedrine and pseudoephedrine was (2.11±0.70) g•L⁻¹; the similarities of all the fingerprints were more than 0.85; there were 10 major common peaks in the fingerprint, including alkaloids, flavonoids and organic acids; the extraction ratio was (17±3.2)%, and the overall transfer rate of ephedrine and pseudoephedrine was (32.4±8.1)%.The method for evaluating the quality of standard decoction of Ephedrae Herba was established in this article, providing reference for the quality control of products which were stemmed from the water extract of Ephedrae Herba.

Study on the Purification Technology of 4 Active Components from Tripterygium wilfordii by Macroporous Resin / 中国药房

OBJECTIVE:To study the purification technology of 4 active components from Tripterygium wilfordii by macropo-rous resin. METHODS:The purification abilities of nine macroporous resins(ADS-5,ADS-8,HPD100,HPD300,HPD400, HPD450,HPD700,HPD722 and HPD750) were studied with the adsorption and desorption rates of triptolide,wilforlide,trip-tonide and tripterine as the index by static adsorption and desorption experiments for 4 active components from T. wilfordii,so as to screen optimal macroporous resins. Using transfer rate of active component as index,single factor test was used to investigate the effects of different sampling method,ratio of mixing sample to total resin quantity,ratio of resin to medicinal material,cleaning so-lution(type,amount and cleaning flow rate),diameter- height ratio of resins,eluant(volume,flow rate)on adsorption,so as to determine the optimal elution technology;validation test was also conducted. RESULTS:HPD722 macroporous resin was chosen as adsorption resin;ratio of diameter to height was 1∶10,resin-medicinal material ratio was 1∶2,and ratio of mixing sample to to-tal resin quantity was 1∶10;wet column installing and mixing resin for sample loading were adopted. The macroporous resin was washed with 12 BV 20%ethanol at the rate of 12 BV/h,and then eluted with 12 BV 95%ethanol at the rate of 6 BV/h. The verifi-cation test results showed that the total transfer rate of 4 active components from T. wilfordii was more than 90%(RSD=0.99%, n=3). CONCLUSIONS:The optimized technology is stable and feasible,and suitable for the purification of 4 active components from T. wilfordii.

Analysis on transfer rate change of heavy metal in decoction and precipitation of Curcuma phaeocaulis before and after processing with vinegar based on ICP-MS / 中国中药杂志

Chinese herbs are mostly used to make decoction, which would form precipitation after standing for cooling and abandoned by patients. Processing with vinegar can change the property of the herbal pieces, such as the transfer rate of heavy metal into decoction. To analyze the transfer rate change of heavy metal in the decoction and precipitation of Curcuma phaeocaulis before and after processing with vinegar, inductively coupled plasma mass spectrometry (ICP-MS) was used to establish the determination method on five heavy metals in C. phaeocaulis, including Copper (Cu), arsenic (As), chromium (Cd), lead (Pb), mercury (Hg), using microwave to digest the samples, indium (In) as the internal standard, and national level standard material tea leaves GBW10016 (GSB-7 tea) as the quality control standard material. Then, the content of five heavy metals in the herbal pieces, decoction and five heavy metals of 6 representative batches of C. phaeocaulis and their vinegar-processing products was determinated. After computation, the transfer rates of heavy metals in the decoction and precipitation of C. phaeocaulis Val. before and after the processing with vinegar were obtained. The results showed that, after the processing with vinegar, total transfer rate of Pb and Hg was decreased significantly; total transfer rate of Cd and Cu was slightly decreased; total transfer rate of As was slightly increased, however heavy metals in all the precipitation were decreased. The results indicated that processing with vinegar had certain influence on heavy metal transfer rate, with certain synergistic and attenuated effect.

Detecção da tolerância de diferentes espécies de capim-colchão a herbicidas inibidores do fotossistema II utilizando a técnica da fluorescência / Detection of crabgrass species tolerance to photosystem II inhibitor herbicides using fluorescence technique

Este estudo teve como objetivo investigar a tolerância ou susceptibilidade das espécies de capim-colchão (Digitaria ciliaris, D. horizontalis e D. nuda) a herbicidas inibidores do fotossistema II (FSII), por meio da técnica da fluorescência, utilizando a taxa de transferência de elétrons do FSII como indicador. Para isso, foi conduzido um experimento em esquema fatorial 3x6, com três espécies de capim-colchão e seis tratamentos (ametryn, hexazinone, diuron+hexazinone, amicarbazone, diuron, tebuthiuron e testemunha) aplicados em pós-emergência. Foi monitorada a taxa de transporte de elétrons (ETR) do FSII em intervalos de tempo crescente e aferida a massa seca das plantas aos 21 dias após a aplicação. A partir dos dados da ETR, calculou-se um valor numérico representativo da taxa de inativação da ETR. Os resultados demonstraram que todas as espécies de capim-colchão estudadas são susceptíveis aos herbicidas ametryn e hexazinone (valores da taxa de inativação da ETR superiores a 10.000). Os herbicidas diuron e tebuthiuron apresentaram menores taxas de inativação da ETR para a D. nuda (3.585 e 3.497, respectivamente) e maiores para as espécies D. ciliaris e D. horizontalis (acima de 10.000), enquanto que o herbicida amicarbazone apresentou valor intermediário para D. nuda (7.967). O monitoramento da ETR foi eficiente para verificar a atuação dos herbicidas nas diferentes espécies estudadas.

This study aimed to investigate the tolerance or susceptibility of crabgrass species (Digitaria ciliaris, D. horizontalis and D. nuda) to herbicides that target photosystem II (PSII), by fluorescence technique using the electron transport rate (ETR) through PSII as an indicator. An experiment was conducted under a factorial arrange (3x6), with three species of crabgrass and six treatments (ametryn, hexazinone, diuron+hexazinone, amicarbazone, diuron, tebuthiuron and control) applied in post-emergence. The ETR through PSII was monitored over time and the plants dry weight measured at 21 days after application. A numerical value of the ETR inactivation was calculated from the data collected. The results showed that the three crabgrass species studied are susceptible to ametryn and hexazinone (ETR inactivation value higher than 10,000). Moreover, diuron and tebuthiuron provided lower ETR inactivation for D. nuda (3,585 and 3,497, respectively) and higher rates for D. horizontalis and D. ciliaris (more than 10,000), whereas amicarbazone showed intermediate inactivation rate for D. nuda (7,967). Monitoring the ETR showed to be an efficient form to verify the herbicides performance in the different species studied here.