A new impurity was detected during high performance liquid chromatographic(HPLC) analysis of eslicarbazepine acetate active pharmaceutical ingredient.The structure of unknown impurity was postulated based on liquid ch...A new impurity was detected during high performance liquid chromatographic(HPLC) analysis of eslicarbazepine acetate active pharmaceutical ingredient.The structure of unknown impurity was postulated based on liquid chromatography mass spectrometry using electrospray ionization and ion trap analyzer(LC/ESI-IT/MS) analysis.Proposed structure of impurity was unambiguously confirmed by synthesis followed by characterization using ~1H,^(13)C nuclear magnetic resonance spectrometry(NMR),~1H-~1H correlation spectroscopy(COSY) and infrared spectroscopy(IR).Based on the spectroscopic and spectrometric data,unknown impurity was characterized as 5-carbamoyl-10,11-dihydro-5H-dibenzo[b,f]azepin-10-yl propionate.展开更多
A new bicadmium(??) complex [Cd2L](ClO4)2?1.25H2O (C28H35Cd2Cl4N6O13.25) was synthesized and characterized by X-ray diffraction and ES mass spectral analyses. It crystallizes in the triclinic system, space group P1 wi...A new bicadmium(??) complex [Cd2L](ClO4)2?1.25H2O (C28H35Cd2Cl4N6O13.25) was synthesized and characterized by X-ray diffraction and ES mass spectral analyses. It crystallizes in the triclinic system, space group P1 with a = 15.630(3), b = 15.990(3), c = 16.330(3) ?, α = 89.90(3), β = 68.87(3), γ = 87.94(3)o, V = 3804.1(13) ?3, Mr = 1034.22, Z = 4, F(000) = 2060, Dc = 1.806 g/cm3, T = 293(2) K, μ = 1.468 mm-1 and λ = 0.71073 ?. The structure was refined to R = 0.0779 and wR = 0.1960 for 7034 observed reflections with I > 2σ(I).展开更多
Hepatitis B virus(HBV)-induced liver failure is an emergent liver disease leading to high mortality.The severity of liver failure may be reflected by the profile of some metabolites.This study assessed the potential o...Hepatitis B virus(HBV)-induced liver failure is an emergent liver disease leading to high mortality.The severity of liver failure may be reflected by the profile of some metabolites.This study assessed the potential of using metabolites as bio- markers for liver failure by identifying metabolites with good discriminative performance for its phenotype.The serum samples from 24 HBV-induced liver failure patients and 23 healthy volunteers were collected and analyzed by gas chromatography-mass spectrometry(GC-MS)to generate metabolite profiles.The 24 patients were further grouped into two classes according to the severity of liver failure.Twenty-five commensal peaks in all metabolite profiles were extracted,and the relative area values of these peaks were used as features for each sample.Three algorithms,F-test,k-nearest neighbor(KNN)and fuzzy support vector machine(FSVM)combined with exhaustive search(ES),were employed to identify a subset of metabolites(biomarkers)that best predict liver failure.Based on the achieved experimental dataset,93.62%predictive accuracy by 6 features was selected with FSVM-ES and three key metabolites,glyceric acid,cis-aconitic acid and citric acid,are identified as potential diagnostic bio- markers.展开更多
A study was carried out to determine arsenic species in seafood samples collected from Chinese sea. The information about arsenic species in samples was provided by high performance liquid chromatography-inductively c...A study was carried out to determine arsenic species in seafood samples collected from Chinese sea. The information about arsenic species in samples was provided by high performance liquid chromatography-inductively coupled plasma mass spectrometer (HPLC ICP MS) and electrospray tandem mass spectrometry (ES MS MS). The arsenic species in thirty Chinese edible seafoods, including algae, fish, crab, shrimp, mussels, oysters, and clams popularly ingested by Chinese people as regular foods, were examined in the present report. Arsenosugars were detected in all of the extracted algae samples (1 5—33 8μg·g -1 dry weight) and some shellfish samples (0 018—0 78μg·g -1 wet weight). Arsenobetaine was detected in all of the extracted fish and shellfish samples (0 025—6 604μg·g -1 wet weight). In contrast, inorganic arsenic was only present in the examined fish and shellfish samples, at levels less than 2% of the total arsenic. The study provides information about a possible distribution pattern of arsenic species in seafood products.展开更多
文摘A new impurity was detected during high performance liquid chromatographic(HPLC) analysis of eslicarbazepine acetate active pharmaceutical ingredient.The structure of unknown impurity was postulated based on liquid chromatography mass spectrometry using electrospray ionization and ion trap analyzer(LC/ESI-IT/MS) analysis.Proposed structure of impurity was unambiguously confirmed by synthesis followed by characterization using ~1H,^(13)C nuclear magnetic resonance spectrometry(NMR),~1H-~1H correlation spectroscopy(COSY) and infrared spectroscopy(IR).Based on the spectroscopic and spectrometric data,unknown impurity was characterized as 5-carbamoyl-10,11-dihydro-5H-dibenzo[b,f]azepin-10-yl propionate.
基金This project was supported by the National Natural Science Foundation of China(No.50372028)
文摘A new bicadmium(??) complex [Cd2L](ClO4)2?1.25H2O (C28H35Cd2Cl4N6O13.25) was synthesized and characterized by X-ray diffraction and ES mass spectral analyses. It crystallizes in the triclinic system, space group P1 with a = 15.630(3), b = 15.990(3), c = 16.330(3) ?, α = 89.90(3), β = 68.87(3), γ = 87.94(3)o, V = 3804.1(13) ?3, Mr = 1034.22, Z = 4, F(000) = 2060, Dc = 1.806 g/cm3, T = 293(2) K, μ = 1.468 mm-1 and λ = 0.71073 ?. The structure was refined to R = 0.0779 and wR = 0.1960 for 7034 observed reflections with I > 2σ(I).
基金Project supported by the Postdoctoral Science Foundation of China(No.20070410397)the National Natural Science Foundation of China(No.60705002)the Science and Technology Project of Zhejiang Province,China(No.2005C13026)
文摘Hepatitis B virus(HBV)-induced liver failure is an emergent liver disease leading to high mortality.The severity of liver failure may be reflected by the profile of some metabolites.This study assessed the potential of using metabolites as bio- markers for liver failure by identifying metabolites with good discriminative performance for its phenotype.The serum samples from 24 HBV-induced liver failure patients and 23 healthy volunteers were collected and analyzed by gas chromatography-mass spectrometry(GC-MS)to generate metabolite profiles.The 24 patients were further grouped into two classes according to the severity of liver failure.Twenty-five commensal peaks in all metabolite profiles were extracted,and the relative area values of these peaks were used as features for each sample.Three algorithms,F-test,k-nearest neighbor(KNN)and fuzzy support vector machine(FSVM)combined with exhaustive search(ES),were employed to identify a subset of metabolites(biomarkers)that best predict liver failure.Based on the achieved experimental dataset,93.62%predictive accuracy by 6 features was selected with FSVM-ES and three key metabolites,glyceric acid,cis-aconitic acid and citric acid,are identified as potential diagnostic bio- markers.
文摘A study was carried out to determine arsenic species in seafood samples collected from Chinese sea. The information about arsenic species in samples was provided by high performance liquid chromatography-inductively coupled plasma mass spectrometer (HPLC ICP MS) and electrospray tandem mass spectrometry (ES MS MS). The arsenic species in thirty Chinese edible seafoods, including algae, fish, crab, shrimp, mussels, oysters, and clams popularly ingested by Chinese people as regular foods, were examined in the present report. Arsenosugars were detected in all of the extracted algae samples (1 5—33 8μg·g -1 dry weight) and some shellfish samples (0 018—0 78μg·g -1 wet weight). Arsenobetaine was detected in all of the extracted fish and shellfish samples (0 025—6 604μg·g -1 wet weight). In contrast, inorganic arsenic was only present in the examined fish and shellfish samples, at levels less than 2% of the total arsenic. The study provides information about a possible distribution pattern of arsenic species in seafood products.
