1.Determination of Acetate Content in Hemodialysis Solutions and Dialysis Concentrates by HPLC.
Huadong WANG ; Yue WANG ; Dong LIU ; Xianghui LIU
Chinese Journal of Medical Instrumentation 2025;49(3):350-354
This study establishes a high-performance liquid chromatography (HPLC) method for the determination of acetate content in hemodialysis solutions and dialysis concentrates. In this study, Synergi Polar-RP column is utilized. Phosphate buffered saline (50 mmol/L, pH=2.5) is used as a mobile phase. The flow rate is 1.0 mL/min. The wavelength of detection is 212 nm. Results show that the linear relationship of acetate is good in the range of 0.1~20 mmol/L, r =0.999 9 and the spike recoveries are from 98.9%~99.5%, RSD<0.5% ( n=3). This method can easily and accurately determine the acetate content in hemodialysis solutions and dialysis concentrates, and can be applied to quality control in the production and use of such products.
Chromatography, High Pressure Liquid/methods*
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Acetates/analysis*
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Hemodialysis Solutions/analysis*
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Dialysis Solutions/analysis*
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Renal Dialysis
2.Chemical constituents from ethyl acetate extraction of Prunus mume.
Can-Can WANG ; Wei ZHANG ; De-Ling WU ; Feng-Qing XU ; Jin-Song LIU ; Jin-Wei QIAO
China Journal of Chinese Materia Medica 2020;45(2):347-351
Eight compounds were isolated from the ethyl acetate extraction of Prunus mume by column chromatography. On the basis of physicochemical properties and spectrum analysis, these compounds were identified as isoquercitrin-6″-O-benzoate(1), pinoresinol(2), naringin(3), ethyl-β-D-glucopyranoside(4), astragalin(5), quercetin(6), hypericin(7), and rutin(8). Among them, compound 1 was a new natural product, and compounds 2-5 were isolated from this plant for the first time. In vitro study, compounds 1, 3, 5-8 could significantly increase the cell survival ratio.
Acetates
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Phytochemicals/analysis*
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Plant Extracts/chemistry*
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Prunus/chemistry*
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Solvents
3.Chemical constituents from ethyl acetate-soluble extraction of Valeriana jatamansi.
Sheng LIN ; Peng FU ; Yun-Heng SHEN ; Ji YE ; Zhong-Xiao ZHANG ; Xian-Wen YANG ; Hui-Liang LI ; Run-Hui LIU ; Xi-Ke XU ; Wei-Dong ZHANG
China Journal of Chinese Materia Medica 2018;43(1):100-108
Application of a combination of various chromatographic techniques including column chromatography over silica gel, Sephadex LH-20, macroporous adsorbent resin, and reversed-phase HPLC, led to the isolation of 173 compounds including irdidoids, monoterpenes, sesquiterpenes, triterpenes, lignans, flavonoids, and simple aromatic derivatives from the ethyl acetate-soluble fraction of the whole plants of Valeriana jatamansi(Valerianaceae), and their structures were elucidated by spectroscopic methods including 1D, 2D NMR UV, IR, and MS techniques. Among them, 77 compounds were new. In previous reports, we have described the isolation, structure elucidation, and bioactivities of 68 new and 25 known compounds. As a consequence, we herein reported the isolation and structure elucidation of the remaining 9 new and 71 known compounds, the structure revision of valeriotriate A(8a), as well as cytotoxicity of some compounds.
Acetates
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Chromatography, High Pressure Liquid
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Flavonoids
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analysis
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Iridoids
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analysis
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Lignans
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analysis
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Molecular Structure
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Monoterpenes
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analysis
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Phytochemicals
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analysis
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Plant Extracts
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chemistry
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Sesquiterpenes
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analysis
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Triterpenes
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analysis
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Valerian
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chemistry
4.Synergistic Anti-bacterial Effects of Phellinus baumii Ethyl Acetate Extracts and beta-Lactam Antimicrobial Agents Against Methicillin-Resistant Staphylococcus aureus.
Seung Bok HONG ; Man Hee RHEE ; Bong Sik YUN ; Young Hoon LIM ; Hyung Geun SONG ; Kyeong Seob SHIN
Annals of Laboratory Medicine 2016;36(2):111-116
BACKGROUND: The development of new drugs or alternative therapies effective against methicillin-resistant Staphylococcus aureus (MRSA) is of great importance, and various natural anti-MRSA products are good candidates for combination therapies. We evaluated the antibacterial activities of a Phellinus baumii ethyl acetate extract (PBEAE) and its synergistic effects with beta-lactams against MRSA. METHODS: The broth microdilution method was used to determine the minimal inhibitory concentration (MIC) and minimal bactericidal concentration (MBC) of the PBEAE. The PBEAE synergistic effects were determined by evaluating the MICs of anti-staphylococcal antibiotic mixtures, with or without PBEAE. Anti-MRSA synergistic bactericidal effects of the PBEAE and beta-lactams were assessed by time-killing assay. An ELISA was used to determine the effect of the PBEAE on penicillin binding protein (PBP)2a production. RESULTS: The MICs and MBCs of PBEAE against MRSA were 256-512 and 1,024-2,048 microg/mL, respectively. The PBEAE significantly reduced MICs of all beta-lactams tested, including oxacillin, cefazolin, cefepime, and penicillin. However, the PBEAE had little or no effect on the activity of non-beta-lactams. Time-killing assays showed that the synergistic effects of two beta-lactams (oxacillin and cefazolin) with the PBEAE were bactericidal in nature (Deltalog10 colony forming unit/mL at 24 hr: 2.34-2.87 and 2.10-3.04, respectively). The PBEAE induced a dose-dependent decrease in PBP2a production by MRSA, suggesting that the inhibition of PBP2a production was a major synergistic mechanism between the beta-lactams and the PBEAE. CONCLUSIONS: PBEAE can enhance the efficacy of beta-lactams for combined therapy in patients infected with MRSA.
Acetates/chemistry
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Agaricales/*chemistry/metabolism
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Anti-Infective Agents/chemistry/*pharmacology
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Drug Synergism
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Enzyme-Linked Immunosorbent Assay
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Methicillin-Resistant Staphylococcus aureus/*drug effects/metabolism
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Microbial Sensitivity Tests
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Penicillin-Binding Proteins/analysis/metabolism
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Plant Extracts/chemistry/*pharmacology
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beta-Lactams/*pharmacology
5.Expression analyses of BcUGT3 and BcUGT6, and their in vitro expression in Escherichia coli.
Yun-Wen TAO ; Jie-Sen XU ; Jing SUN ; Jian-He WEI ; Juan LIU ; Chun SUI
China Journal of Chinese Materia Medica 2014;39(2):185-191
The tissue-specific and MeJA-induced transcriptional levels of BcUGT3 and BcUGT6 in Bupleurum chinense were analyzed in the present study. The transcriptional levels of BcUGT3 in root, leaf, flower and fruit were similar and they all were higher than those in stem. The transcriptional level of BcUGT6 was the highest in leaf and the lowest in flower among in all tested tissues. With non-treated adventitious roots as control, BcUGT6's transcriptional levels were elevated to nearly 2 folds for 2 h, 8 h, 24 h, 2 d and 4 d in MeJA-treated adventitious roots of B. chinense. It showed that the transcriptional level of BcUGT6 was slightly affected by MeJA. While, BcUGT3's transcriptional levels were gradually elevated, and till 4 d after MeJA treatment, the expression level was about 7 folds than that of non-treated control. Using pET-28a (+), the expressions of two genes was investigated. Induced by IPTG, the target proteins were expressed in E. coli and then purified. All the results obtained in the present study will be helpful for follow-up bio-function analysis of BcUGT3 and BcUGT6.
Acetates
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pharmacology
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Bupleurum
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cytology
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enzymology
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genetics
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Cell Membrane
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metabolism
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Cyclopentanes
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pharmacology
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Escherichia coli
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genetics
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Gene Expression
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Gene Expression Regulation, Plant
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drug effects
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Hexosyltransferases
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chemistry
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genetics
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isolation & purification
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metabolism
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Intracellular Space
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metabolism
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Oxylipins
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pharmacology
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Protein Sorting Signals
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Protein Structure, Secondary
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Protein Transport
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Sequence Analysis
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Transcription, Genetic
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drug effects
6.Technological parameter optimization method for washing of coarse bear gall powder extracts based on NIR spectroscopy.
Wen-Long LI ; Shao-Yong LIU ; Dong-Sheng XUE ; Zhi-Wei CHENG ; Hai-Bin QU
China Journal of Chinese Materia Medica 2014;39(1):75-79
During the washing process of coarse bear gall powder extracts, it is necessary to adjust the amount of ethyl acetate according to the properties of raw materials, which aims to improving the yield and purity of the final product. In the research, using NIR spectra to reflect the comprehensive properties of coarse bear gall powder extracts, the process is optimized in a flexible way. Forty batches experiments are designed according to the weight ratio of ethyl acetate and coarse extracts of bear gall powder. The NIR spectra of the coarse extracts of bear gall powder are collected and processed using principal component analysis (PCA) method. The first 8 principal components combined with the amount of the ethyl acetate are used as the input variables, and calibration models are established to predict the yield and purity of the final product 30 batches are used as calibration set, which is used to establish the models, and other 10 batches are used as validation set, which is used for the performance appraisal of the established models. The correlation coefficients of the calibration, inner cross-validation and external validation for the purity model are 0.902, 0.896 and 0.883, respectively, and the RMSEC, RMSECV and RMSEP are 1.22%, 1.48% and 1.59%, respectively. The correlation coefficients of the calibration, inner cross-validation and external validation for the yield model are 0.921, 0.859 and 0.916, respectively, and the RMSEC, RMSECV and RMSEP are 1.39%, 1.65% and 1.53% respectively. This work demonstrated that NIR spectra combined with technology parameter could be used to predict the yield and purity of the final product. Using the established models, the most appropriate amount of the ethyl acetate can be determined according to the properties of the coarse bear gall powder extracts, and the yield and purity of the final product can be improved.
Acetates
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chemistry
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Animals
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Gallbladder
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chemistry
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Medicine, Chinese Traditional
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Powders
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chemistry
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Principal Component Analysis
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methods
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Spectroscopy, Near-Infrared
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methods
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Ursidae
7.Determination of the content of residual solvents in Haikesu 2 by head-space gas chromatography.
Xuan XIAO ; Dong LIU ; Ke-Min WANG ; Jia-Zhi CHEN ; Shu ZHANG
Acta Academiae Medicinae Sinicae 2014;36(6):602-605
OBJECTIVETo determine ethylacetate and petroleum ether(60-90 ℃)in Haikesu 2,which is one of the raw materials of artificial musk,using the head-space gas chromatography.
METHODSThe determination was performed on HP-5(30 m×0.53 mm,5 Μm)capillary column with an hydrogen flame ionization detector. The solvent was dimethyl sulfoxide and the internal standard was methanol. The injector temperature and the detector temperature were controlled at 180 ℃ and 250 ℃,respectively. The carrier gas was nitrogen. The containers of head-space injector were preheated at 90 ℃ for 15 minutes. The column temperature was programmed raised,which achieved baseline separation of the components.
RESULTSThe results showed a good linear relationship for ethylacetate and petroleum ether(60-90 ℃)in their linearity range;and the limit of detection was 0.7 and 0.3 Μg/ml,respectively. The good precision and good average recoveries were satisfactory.
CONCLUSIONThe head-space gas chromatography is simple,rapid,and precise technique for the measurement of residual solvents in Haikesu 2.
Acetates ; analysis ; Chromatography, Gas ; Drugs, Chinese Herbal ; chemistry ; Fatty Acids, Monounsaturated ; chemistry ; Flame Ionization ; Solvents ; analysis
8.Effects of methyl jasmonate on accumulation and release of main tropane alkaloids in liquid cultures of Datura stramonium hairy root.
Ji-Wei SUN ; Hong ZHANG ; Feng-Ying WANG ; Yi-Ming SUN ; Min SUN
China Journal of Chinese Materia Medica 2013;38(11):1712-1718
OBJECTIVETo study the effects of methyl jasmonate (MJ) on the accumulation and release of main secondary metabolites i. e. scopolamine and hyoscyamine in liquid cultures of Datura stramonium hairy roots.
METHODAfter 18 days liquid culture of D. stramonium hairy roots induced by agrobacterium rhizogenes C58C1, the chemical elicitor methyl jasmonate was added into 1/2 MS liquid cultures and scopolamine and hyoscyamine on the day 0, 3, 6, 9 and 12, after dealing with MJ, was determined by HPLC.
RESULTAfter dealing with MJ on the day 3, 6, 9 and 12,the concentration of scopolamine reached to 0.419, 0.439, 0.431, 0.374 mg x g(-1), respectively, the increase of scopolamine were 1.36, 1.42, 1.17 and 1.12 fold higher than that of the control, respectively. And hyoscyamine reached 1.493, 0.817, 0.723 and 0.698 mg x g(-1), respectively, the increase of hyoscyamine were 2.28, 1.11, 0.63 and 0.70 fold higher than that of the control, respectively.
CONCLUSIONMJ could stimulate the accumulation of scopolamine and hyoscyamine (3,6 d) in D. stramonium hairy root and have released them into the culture medium.
Acetates ; pharmacology ; Alkaloids ; analysis ; metabolism ; Cell Culture Techniques ; Cyclopentanes ; pharmacology ; Datura stramonium ; chemistry ; drug effects ; growth & development ; metabolism ; Oxylipins ; pharmacology ; Plant Roots ; chemistry ; drug effects ; growth & development ; metabolism ; Tropanes ; analysis ; metabolism
9.Effect of montelukast on the expression of neurokinin-1 receptor in young asthmatic rats with airway remodeling.
Bing WEI ; Yun-Xiao SHANG ; Miao LI ; Han ZHANG
Chinese Journal of Contemporary Pediatrics 2013;15(4):298-301
OBJECTIVETo investigate the effect of montelukast on the expression of sensory neuropeptide (neurokinin-1) receptor (NK1R) in young asthmatic rats with airway remodeling.
METHODSTwenty-four Sprague-Dawley rats were randomly divided into control group (n=8), asthma (n=8), and montelukast groups (n=8). A rat model of asthma was induced by ovalbumin (OVA) inhalation. Normal saline was used instead of sensitizing solution and 1% OVA in the control group. Each rat in the montelukast group was given montelukast (15 mg/kg) by gavage 2 h before OVA inhalation. All rats received their respective treatments for 8 weeks. Immunohistochemistry, real-time PCR and Western blot were used to measure the mRNA and protein expression levels of NK1R in asthmatic airway remolding and to evaluate the effect of montelukast on NK1R expression.
RESULTSThe asthma group showed significantly higher mRNA and protein expression levels of NK1R than the control group (P<0.01). The mRNA and protein expression levels of NK1R in the montelukast group were significantly lower than in the asthma group (P<0.05), but significantly higher than in the control group (P<0.01).
CONCLUSIONSRats with induced asthma have upregulated NK1R expression in the airway, and montelukast can downregulate NK1R expression during airway remodeling.
Acetates ; pharmacology ; Airway Remodeling ; drug effects ; Animals ; Anti-Asthmatic Agents ; pharmacology ; Asthma ; drug therapy ; metabolism ; Female ; Leukotriene Antagonists ; pharmacology ; Quinolines ; pharmacology ; RNA, Messenger ; analysis ; Rats ; Rats, Sprague-Dawley ; Receptors, Neurokinin-1 ; analysis ; genetics
10.HPLC fingerprint of ethyl acetate extraction of Saxifraga stolonifera.
Mei ZHOU ; Hua-Guo CHEN ; Chun XIAN ; Zhi-Jin HUANG ; Xin ZHOU
China Journal of Chinese Materia Medica 2013;38(7):1026-1029
OBJECTIVETo establish an HPLC fingerprint of ethyl acetate extraction of Saxifraga stolonifera.
METHODThe HPLC analysis was performed on a Diamonsil C18 (4.6 mm x 250 mm, 5 microm) column with isocratic elution of acetonitrile-0.05% phosphoric acid at a flow rate of 1.0 mL x min(-1). The detection wavelength was set at 256 nm and the column temperature was set at 30 degrees C.
RESULTThe HPLC fingerprint of ethyl acetate extraction of S. stolonifera has been established. There were fifteen common peaks, seven of which were identified by reference substances. The RSD of relative retention time was less than 3% in the precision and repeated tests. Eleven samples from different area can be distinguished from their fingerprints.
CONCLUSIONThis method is reasonable and reliable and can be used for quality control of S. stolonifera.
Acetates ; Chromatography, High Pressure Liquid ; methods ; Drugs, Chinese Herbal ; analysis ; standards ; Quality Control ; Saxifragaceae ; chemistry

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