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
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 gro...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
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 liqui...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, 13C nuclear magnetic resonance spectrometry （NMR）, 1H-1H correlation spectro-scopy （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
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.
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).
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, 13C nuclear magnetic resonance spectrometry （NMR）, 1H-1H correlation spectro-scopy （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.
