1.Quantitative determination of voglibose contents in its tablets with high-performance liquid chromatography-mass spectrometry.
Xiang-qun ZHANG ; Ling-hua WU ; Fang-jun CHEN ; Yi ZHANG ; Lu CHEN
Journal of Zhejiang University. Medical sciences 2014;43(2):141-144
OBJECTIVETo develop a method for determination of voglibose contents in its tablets by high-performance liquid chromatography-mass spectrometry (HPLC-MS).
METHODSThe measurements were carried out on an Agilent ZORBAX Eclipse Plus C18 column (2.1×150mm 3.2μm) with a temperature of 40 degrees Celsius. A mixture of methanol and water (2:3,v/v) was used as a mobile phase at a flow rate of 0.25 ml/min. Voglibose was detected in an electrospray ionization (ESI) mode with MRM.
RESULTSThe calibration curves of voglibose showed good linearity in a range of 1.5804-2.6340 μg/ml (r=0.9990). The average recovery was 100.2% with RSD of 1.37% (n=6) for m/z 268.2/74.2.Linearity was obtained with r=0.9976 and the average recovery was 99.3% with RSD of 1.78% (n=6) for m/z 268.2/92.2.
CONCLUSIONHPLC-MS method is accurate,reproducible and can be used for quality control of voglibose tablets.
Chromatography, High Pressure Liquid ; methods ; Inositol ; analogs & derivatives ; analysis ; Mass Spectrometry ; methods ; Tablets
2.Isolation and identification of chemical constituents from Taxus cuspidta Sibe et Zucc.
Di WU ; Ya-Nan LI ; Li-Jun WU ; Hui-Yuan GAO
Acta Pharmaceutica Sinica 2010;45(11):1398-1401
Three compounds were isolated from the extract of Taxus cuspidta Sibe et Zucc with the column chromatography on silica gel and preparative HPLC methods. Their structures were identified according to the physicochemical properties and spectral analysis, and they were identified as (E)-1-methoxy-2-O-(p-coumaroyl)-myo-inositol (1), 2-deacetoxy-7beta, 9a, 10beta-trideacetyltaxinine J (2) and (3aS, 4aR, 6S, 8S, 8aS, 9R, 10R, 10aS)-benz[f]azulene-6, 8, 9, 10 (3H)-terol, 3a, 4, 4a, 5, 6, 7, 8, 8a, 9, 10-decahydro-10a-(1-hydroxyl-1-methylethyl)-1, 8a-dimethyl-5-methylene (3). Among them, compound 1 was a new compound, and compounds 2, 3 were two novel natural products.
Azulenes
;
chemistry
;
isolation & purification
;
Coumarins
;
chemistry
;
isolation & purification
;
Inositol
;
analogs & derivatives
;
chemistry
;
isolation & purification
;
Molecular Structure
;
Plants, Medicinal
;
chemistry
;
Taxoids
;
chemistry
;
isolation & purification
;
Taxus
;
chemistry
3.Proton magnetic resonance spectroscopy of normal human brain and glioma: a quantitative in vivo study.
Zhi-yong TONG ; Yamaki TOSHIAKI ; Yun-jie WANG
Chinese Medical Journal 2005;118(15):1251-1257
BACKGROUNDIn vivo proton magnetic resonance spectroscopy (MRS) provides a noninvasive method of examining a wide variety of cerebral metabolites in both healthy subjects and patients with various brain diseases. Absolute metabolite concentrations have been determined using external and internal standards with known concentrations. When an external standard is placed beside the head, variations in signal amplitudes due to B1 field inhomogeneity and static field inhomogeneity may occur. Hence an internal standard is preferable. The purpose of this study was to quantitatively analyze the metabolite concentrations in normal adult brains and gliomas by in vivo proton MRS using the fully relaxed water signal as an internal standard.
METHODSBetween January 1998 and October 2001, 28 healthy volunteers and 16 patients with gliomas were examined by in vivo proton MRS. Single-voxel spectra were acquired using the point-resolved spectroscopic pulse sequence with a 1.5 T scanner (TR/TE/Ave = 3000 ms/30 ms/64).
RESULTSThe calculated concentrations of N-acetyl-asparatate (NAA), creatine (Cre), choline (Cho), and water (H2O) in the normal hemispheric white matter were (23.59 +/- 2.62) mmol/L, (13.06 +/- 1.8) mmol/L, (4.28 +/- 0.8) mmol/L, and (47,280.96 +/- 5414.85) mmol/L, respectively. The metabolite concentrations were not necessarily uniform in different parts of the brain. The concentrations of NAA and Cre decreased in all gliomas (P < 0.001). The ratios of NAA/Cho and NAA/H2O showed a significant difference between the normal brain and gliomas, and also between the high and low grades (P < 0.001).
CONCLUSIONSQuantitative analysis of in vivo proton MR spectra using the fully relaxed water signal as an internal standard is useful. The concentrations of NAA and the ratios of NAA/H2O and NAA/Cho conduce to discriminating between the glioma and normal brain, and also between the low-grade glioma and high-grade glioma.
Adult ; Aspartic Acid ; analogs & derivatives ; metabolism ; Brain ; metabolism ; Choline ; metabolism ; Creatine ; metabolism ; Female ; Glioma ; metabolism ; Glycine ; metabolism ; Humans ; Inositol ; metabolism ; Magnetic Resonance Spectroscopy ; Male
4.1H-proton magnetic resonance spectroscopy in patients with multiple system atrophy and cognitive dysfunction.
Xiaoshuang XIANG ; Xuan HOU ; Zhanfang SUN ; Gaofeng ZHOU ; Beisha TANG ; Hong JIANG
Journal of Central South University(Medical Sciences) 2015;40(6):639-645
OBJECTIVE:
To detect metabolic changes of bilateral frontal lobe in patients with multiple system atrophy (MSA) and cognitive dysfunction by 1H-proton magnetic resonance spectroscopy (1H-MRS).
METHODS:
N-acetylaspartate (NAA)/creatine(Cr), choline (Cho)/Cr, myoinositol (mI)/Cr in three sides of frontal lobe were detected by 1H-MRS in 48 healthy controls, 23 patients with MSA and cognitive dysfunction and 19 patients with MSA but without cognitive dysfunction.
RESULTS:
NAA/Cr of bilateral frontal lobes in patients with MSA and cognitive dysfunction was significantly decreased compared with MSA patients without cognitive dysfunction and healthy controls (P<0.05). mI/Cr of right frontal lobes was significantly increased in patients with MSA and cognitive dysfunction compared with healthy controls (P<0.05). There was a negative correlation between NAA/Cr of bilateral frontal lobes and duration while a positive correlation between NAA/Cr of bilateral frontal lobes and MoCA score in patients with MSA and cognitive dysfunction.
CONCLUSION
There is a decrease in NAA/Cr and an increase in mI/Cr in frontal lobes in patients with MSA and cognitive dysfunction, which may be associated with cognitive dysfunction in MSA patients.
Aspartic Acid
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analogs & derivatives
;
metabolism
;
Choline
;
metabolism
;
Cognition Disorders
;
physiopathology
;
Creatine
;
metabolism
;
Frontal Lobe
;
metabolism
;
Humans
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Inositol
;
metabolism
;
Multiple System Atrophy
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physiopathology
;
Proton Magnetic Resonance Spectroscopy
5.Development and validation of HPLC-UV-MS method for the control of four anti-diabetic drugs in suspected counterfeit products.
Xiu-mei DAI ; Ning AN ; Jian-min WU ; Hui-yi LI ; Qi-ming ZHANG
Acta Pharmaceutica Sinica 2010;45(3):347-352
An HPLC-UV method has been developed for the determination of valibose, miglitol, voglibose and acarbose, the four anti-diabetic drugs. The separation was accomplished successfully by using reversed phase chromatography (Prevail carbohydrate column, 250 mm x 4.6 mm, 5 microm) with a gradient acetonitrile-phosphate buffer solution (pH 8.0) at a wavelength of 210 nm. Furthermore, the method of a high-performance liquid chromatography coupled with ESI-MS in positive ionization mode has been established. These two methods were successfully applied to the assay and qualitative detection of four alpha-glucosidase inhibitors in the potential counterfeit anti-diabetic drugs.
1-Deoxynojirimycin
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analogs & derivatives
;
analysis
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Acarbose
;
analysis
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Chromatography, High Pressure Liquid
;
methods
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Chromatography, Reverse-Phase
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Glycoside Hydrolase Inhibitors
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Hypoglycemic Agents
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chemistry
;
Inositol
;
analogs & derivatives
;
analysis
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Spectrometry, Mass, Electrospray Ionization
;
methods
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Spectrophotometry, Ultraviolet
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alpha-Glucosidases
;
analysis
6.Correlation of neurochemical metabolism with memory function in young adult patients with first-episode depression studied with proton magnetic resonance spectroscopy.
Weibo LIU ; Hualiang YU ; Biao JIANG ; Leilei ZHENG ; Shaohua YU ; Bing PAN ; Risheng YU
Journal of Zhejiang University. Medical sciences 2013;42(4):450-455
OBJECTIVETo investigate the correlation of neurochemical metabolism in hippocampus with memory function in young adult patients with first-episode depression.
METHODSTwenty patients with first-episode depression (patient group) and fifteen health subjects (control group) were enrolled in the study. The neurochemical metabolism, including the levels of N-acetylaspartate (NAA), Choline (Cho), Creatine (Cr), Myoinositol (mI) were measured by proton magnetic resonance spectroscope (1H-MRS) in bilateral hippocampus. Wechsler Memory Scale (WMS) were used to examine the memory function in both groups.
RESULTSThe memory quotient (89.15 ±6.62) of patient group was significantly lower than that of controls (P <0.01),the scores of long-term memory,short-term memory and immediate memory in patients were also lower than those of controls (P<0.05 or 0.01). In patient group, the ratio of NAA/Cr (1.34 ±0.08) in the left hippocampus was significantly lower than that of control group (P<0.01); and the ratio of mI/Cr in the bilateral hippocampus [(0.63 ±0.13) in left and (0.6 ±0.1) in right] was significantly higher than those in control group (P<0.05). In patient group,the ratio of NAA/Cr in the left hippocampus was positively correlated with WMS scores (P<0.01), and the ratio of mI/Cr in the left hippocampus was negatively correlated with WMS scores (P<0.05).
CONCLUSIONThe memory deficit and abnormal metabolism function of neuron cell in hippocampus coexist in young adult patients with first-episode depression, and the lower NAA/Cr and higher mI/Cr ratio in the left hippocampus may result in the memory deficit.
Adolescent ; Adult ; Aspartic Acid ; analogs & derivatives ; metabolism ; Case-Control Studies ; Creatine ; metabolism ; Depressive Disorder ; metabolism ; physiopathology ; Female ; Hippocampus ; metabolism ; Humans ; Inositol ; metabolism ; Magnetic Resonance Spectroscopy ; Male ; Memory ; Neuropsychological Tests ; Young Adult
7.1H NMR based metabonomics study on the antidepressant effect of genipin in rat hippocampus.
Guo-Jiang PENG ; Bi-Yun SHI ; Jun-Sheng TIAN ; Shan GAO ; Xue-Mei QIN
Acta Pharmaceutica Sinica 2014;49(2):209-216
The purpose of this study is to explore depression metabolic markers in rat hippocampus and to investigate the anti-depressant effect of genipin and its mechanisms using nuclear magnetic resonance (NMR) metabonomics. Chronic unpredictable mild stress (CUMS) procedure was conducted to establish the depressive rat model. At the beginning of the third week, genipin low dose (25 mg x kg(-1)), middle dose (50 mg x kg(-1)), high dose (100 mg x kg(-1)), and venlafaxine (50 mg x kg(-1)) were given to the CUMS rats separately once daily for two weeks except control and model groups. Rat hippocampus was analyzed by 1H NMR based metabonomics after drug administration for 2 weeks. Significant differences in the metabolic profile of rat hippocampus of the CUMS treated group and the control group were observed with metabolic effects of CUMS including decreasing in glycine and N-acetylaspartate, increasing in inositol, glutamate, lactate, glutamine, taurine and alanine. Genipin showed ideal antidepressive effects at a dose of 50 mg x kg(-1) in rats, decrease of inositol, glutamate, lactate, alanine were observed, while glycine and N-acetylaspartate were increased. Important influence has been found on normal nervous system function of these significant changed metabolites, which suggests that the antidepressant effect of genipin may be played by enhancing the activity of neurons in hippocampus, repairing and improving the function of the neuron. The metabonomics approach is an effective tool for the investigation of the anti-depressant effect and pharmacologic mechanisms of genipin.
Alanine
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metabolism
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Animals
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Antidepressive Agents
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isolation & purification
;
pharmacology
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Aspartic Acid
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analogs & derivatives
;
metabolism
;
Behavior, Animal
;
drug effects
;
Chronic Disease
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Depression
;
drug therapy
;
metabolism
;
physiopathology
;
Gardenia
;
chemistry
;
Glutamic Acid
;
metabolism
;
Glycine
;
metabolism
;
Hippocampus
;
drug effects
;
metabolism
;
Inositol
;
metabolism
;
Iridoids
;
isolation & purification
;
pharmacology
;
Lactic Acid
;
metabolism
;
Magnetic Resonance Spectroscopy
;
Male
;
Metabolomics
;
Plants, Medicinal
;
chemistry
;
Rats
;
Rats, Sprague-Dawley
8.Effects of 11, 12-epoxyeicosatrienoic acid preconditioning and postconditioning on Ca(2+)- handling proteins in myocardial ischemia/reperfusion injury in rats.
Yan-Xia WANG ; Xiang-Jun ZENG ; Ling-Qiao LU ; Li-Quan MA ; Dong-Qiao JIANG ; Jing MU ; Xiao-Yan WANG ; Li-Ke ZHANG ; Chao-Shu TANG ; Gang HAO
Acta Academiae Medicinae Sinicae 2007;29(6):787-791
OBJECTIVETo investigate the effects of 11, 12-epoxyeicosatrienoic acid (11, 12-EET) preconditioning and postconditioning on Ca(2+)-handling proteins in myocardial ischemia/reperfusion (IR) injury in rats and reveal the effects and mechanism of 11, 12-EET on cardioprotection. METHODS The IR injury model was built by stopping perfusion for 40 minutes followed by reperfusion for 30 minutes. The isolated Langendorff-perfused rat hearts were divided into 4 groups: control group, IR group, EET preconditioning (Pre-EET) group and EET postconditioning (Post-EET) group. The computer-based electrophysiological recorder system was used to measure the changes of the maximal rate of pressure increased in the contraction phase (+dp/dt(max)), the maximal rate of pressure decreased in the diastole phase (-dp/dt(max)), the left ventricular end diastolic pressure (LVEDP) and the difference of left ventricular pressure (delta LVP). The activity of Ca(2+)-ATPase in sarcoplasmic reticulum was measured with colorimetric method. Reverse transcription-polymerase chain reaction was used to assess the gene expression of C(a2+)-handling protein [sarcoplasic reticulum Ca(2+)-ATPase (SERCA), phospholamban (PLB), ryanodine receptor type 2 (RyR,), and 1, 4, 5-trisphosphate inositol receptor type 2 (IP3 R2) ] mRNAs level.
RESULTSCompared with IR group, the myocardial functions, the value of Ca(2+)-ATPase, and the expressions of IP3 R2 mRNA were significantly increased and the expression of PLB mRNA was significantly decreased in both Pre-EET group and Post-EET group (P < 0.05, P < 0.01). And the expression of SERCA mRNA was significantly increased in Pre-EET group (P < 0. 05). However, no significant differences were detected between Pre-EET and Post-EET groups. Moreover, the expression of RyR2 mRNA was not significantly different among all groups.
CONCLUSIONS11, 12-EET preconditioning and post-conditioning can protect myocardium from IR injury by elevating the activity of Ca(2+)-ATPase in sarcoplasmic reticulum, up-regulating the expression of IP3 R2 mRNA, and down-regulating the expression of PLB mRNA. Moreover, up-regulating the expression of SERCA mRNA maybe one of mechanisms of 11, 12-EET preconditioning on cardio protection against IR injury.
8,11,14-Eicosatrienoic Acid ; analogs & derivatives ; pharmacology ; Animals ; Calcium-Binding Proteins ; drug effects ; metabolism ; Inositol 1,4,5-Trisphosphate Receptors ; drug effects ; metabolism ; Ischemic Preconditioning, Myocardial ; methods ; Myocardial Reperfusion Injury ; metabolism ; prevention & control ; Rats ; Ryanodine Receptor Calcium Release Channel ; metabolism ; Sarcoplasmic Reticulum Calcium-Transporting ATPases ; drug effects ; metabolism
9.Assessment of therapeutic effect of losartan on diabetes mellitus with gas chromatography-based metabonomics.
Kai-Long YUAN ; Xian-Zhe SHI ; Xin LU ; Peng GAO ; Guo-Wang XU
Acta Academiae Medicinae Sinicae 2007;29(6):719-724
OBJECTIVETo assess the therapeutic effect of losartan on type 2 diabetes mellitus (DM2) with gas chromatography (GC)-based metabonomics.
METHODSDM2 patients were dosed with losartan (100 mg/d) and urines were collected at week 8 and 12. The biochemical criteria (blood pressure, urinary albumen, urinary 8-hydroxy-2'-deoxyguanosine and blood creatinine) were analyzed. Urine samples were derivatived and analyzed by GC. Multivariate metabonomics analysis was performed after peak alignment.
RESULTSAfter 8-12 weeks, losartan showed little curative effect and no remarked changes of biochemical criteria were observed. However, metabonomics analysis revealed that some biomarkers such as glucitol and inositol changed.
CONCLUSIONGC-based metabonomics analysis enables the rapid identification of metabolic differences and provides information concerning therapeutic effect of losartan.
Albuminuria ; urine ; Biomarkers ; blood ; chemistry ; urine ; Chromatography, Gas ; methods ; Creatinine ; blood ; Deoxyguanosine ; analogs & derivatives ; urine ; Diabetes Mellitus ; drug therapy ; Diabetes Mellitus, Type 2 ; drug therapy ; Drug Monitoring ; Humans ; Hypoglycemic Agents ; therapeutic use ; Inositol ; chemistry ; Losartan ; therapeutic use ; Metabolome ; drug effects ; Sorbitol ; chemistry
10.The effects of nonyl phenoxypolyethoxyl ethanol on cell damage pathway gene expression in SK-NSH cells.
Samel PARK ; Il Woong HWANG ; Jin Sheon KIM ; Hyo Chul KANG ; Su Yeon PARK ; Hyo Wook GIL ; Ho Yeon SONG ; Sae Yong HONG
The Korean Journal of Internal Medicine 2015;30(6):873-883
BACKGROUND/AIMS: Most pesticide formulations contain both chief and additive ingredients. But, the additives may not have been tested as thoroughly as the chief ingredients. The surfactant, nonyl phenoxypolyethoxylethanol (NP40), is an additive frequently present in pesticide formulations. We investigated the effects of NP40 and other constituents of a validamycin pesticide formulation on cell viability and on the expression of genes involved in cell damage pathways. METHODS: The effects of validamycin pesticide ingredients on cell viability and of NP40 on the mRNA expression of 80 genes involved in nine key cellular pathways were examined in the human neuroblastoma SK-N-SH cell line. RESULTS: The chemicals present in the validamycin pesticide formulation were cytotoxic to SK-N-SH cells and NP40 showed the greatest cytotoxicity. A range of gene expression changes were identified, with both up- and down-regulation of genes within the same pathway. However, all genes tested in the necrosis signaling pathway were down-regulated and all genes tested in the cell cycle checkpoint/arrest pathway were up-regulated. The median fold-change in gene expression was significantly higher in the cell cycle checkpoint/arrest pathway than in the hypoxia pathway category (p = 0.0064). The 70 kDa heat shock protein 4 gene, within the heat shock protein/unfolded protein response category, showed the highest individual increase in expression (26.1-fold). CONCLUSIONS: NP40 appeared to be particularly harmful, inducing gene expression changes that indicated genotoxicity, activation of the cell death (necrosis signaling) pathway, and induction of the 70 kDa heat shock protein 4 gene.
Aged
;
Cell Cycle Checkpoints/drug effects/genetics
;
Cell Line, Tumor
;
Cell Survival/drug effects
;
Dose-Response Relationship, Drug
;
Female
;
Gene Expression Regulation/drug effects
;
Genes, cdc
;
HSP110 Heat-Shock Proteins/genetics/metabolism
;
Humans
;
Inositol/*analogs & derivatives/chemistry/poisoning
;
Necrosis
;
Neurons/*drug effects/metabolism/pathology
;
Nonoxynol/chemistry/*toxicity
;
Pesticides/chemistry/*poisoning
;
RNA, Messenger/metabolism
;
Signal Transduction/drug effects
;
Surface-Active Agents/chemistry/*toxicity