目的探讨尿液中核酸氧化代谢产物8-oxo-Gsn和8-oxo-d Gsn对HBV感染引起肝损伤程度的评估价值。方法收集笔者医院94例慢性乙型肝炎(以下简称慢乙肝)患者行超声引导下肝穿刺活检前的尿液,95例健康者以及25例乙肝表面携带者的随机尿液,采...目的探讨尿液中核酸氧化代谢产物8-oxo-Gsn和8-oxo-d Gsn对HBV感染引起肝损伤程度的评估价值。方法收集笔者医院94例慢性乙型肝炎(以下简称慢乙肝)患者行超声引导下肝穿刺活检前的尿液,95例健康者以及25例乙肝表面携带者的随机尿液,采用同位素稀释高效液相-串联质谱法(ID-LC-MS/MS)分析尿液中DNA氧化标志物8-oxod Gsn和RNA氧化标志物8-oxo-Gsn,并结合病理结果和生化指标(ALT和AST),分析各指标之间的相关性,通过ROC曲线评估二者对肝损伤程度的预测价值,并分析8-oxo-Gsn和8-oxo-d Gsn在不同炎症活动度和不同纤维化程度患者中的水平差异。结果实验组中,88.5%(46/52)的男性8-oxo-Gsn高于正常对照组,85.7%(36/42)的女性8-oxo-Gsn高于正常对照组;肝脏炎症程度高的患者(G_3~G_4)尿液中RNA氧化标志物8-oxo-Gsn显著高于炎症程度低的患者(G_0~G_2)(4.28 vs 3.26,χ~2=11.117,P=0.009),纤维化程度高的患者8-oxo-Gsn水平也高于纤维化程度低的患者(3.66 vs 3.29),但未达到显著性水平(χ~2=3.626,P=0.323)。尿液中RNA氧化标志物8-oxo-Gsn对肝脏炎症程度有较好的预测价值(敏感度为82.4%,特异性为75%,AUC=0.813),对纤维化程度有较好的预测价值(敏感度为83.3%,特异性为77.1%,AUC=0.824)。结论尿液中RNA氧化标志物8-oxo-Gsn可能是HBV感染引起的肝损伤严重程度的评估指标。展开更多
目的探讨妊娠糖尿病(gestational diabetes mellitus,GDM)患者尿液RNA氧化标志物8G-氧化鸟苷(8-oxo-7,8-dihydroguanosine,8-oxo-Gsn)的水平及与妊娠结局的关系。方法选取2018年2月~2021年2月汉川市中医医院收治的106例GDM患者为观察组...目的探讨妊娠糖尿病(gestational diabetes mellitus,GDM)患者尿液RNA氧化标志物8G-氧化鸟苷(8-oxo-7,8-dihydroguanosine,8-oxo-Gsn)的水平及与妊娠结局的关系。方法选取2018年2月~2021年2月汉川市中医医院收治的106例GDM患者为观察组,根据妊娠结局情况分为妊娠结局良好组和妊娠结局不良组。另选取同期进行体检的90例健康孕妇为对照组。收集所有孕妇的临床资料并进行比较。采用同位素稀释高效液相-串联质谱法(isotope dilution high performance liquid phase-tandem mass spectrometry,ID-LC-MS/MS)分析尿液中8-oxo-Gsn水平。采用ROC曲线评估8-oxo-Gsn对GDM患者不良妊娠结局的评估价值。多因素回归分析影响GDM患者不良妊娠结局的危险因素。结果与对照组相比,观察组尿液8-oxo-Gsn水平(3.89±0.63μmol/mol vs 2.26±0.47μmol/mol)及不良妊娠结局的发生率(29.25%vs 11.11%)明显升高,差异有统计学意义(t=20.225,χ^(2)=9.676,均P<0.05)。与妊娠结局良好组相比,妊娠结局不良组患者尿液8-oxo-Gsn水平(4.67±0.77μmol/mol vs 3.56±0.57μmol/mol)升高,差异有统计学意义(t=8.197,P<0.05)。ROC曲线分析结果显示,8-oxo-Gsn预测GDM患者不良妊娠结局的曲线下面积为0.847,截断值为4.049μmol/mol,敏感度和特异度分别为77.40%,81.30%。HOMA-IR[OR(95%CI):4.726(2.027~11.021)],8-oxo-Gsn[OR(95%CI):5.591(2.239~13.964)]是GDM患者发生不良妊娠结局的独立危险因素(均P<0.05)。结论GDM患者尿液8-oxo-Gsn水平升高,与患者不良妊娠结局有关,且对不良妊娠结局具有较优的预测价值。展开更多
The reaction mechanism of OXO(X=Cl, Br) with H(2\%S\%) was studied theoretically by using the B3LYP/6-311+G(3df, 3pd) and the high-level electron-correlation QCISD(T)/6-311+G ** at single-point. The results show that ...The reaction mechanism of OXO(X=Cl, Br) with H(2\%S\%) was studied theoretically by using the B3LYP/6-311+G(3df, 3pd) and the high-level electron-correlation QCISD(T)/6-311+G ** at single-point. The results show that the mechanism for the title reaction involves three channels, from which OH+XO, HO 2+X and HX+O 2 products could be obtained, respectively. Therefore, the channel to yield the products OH+XO is the dominant one in agreement with the experiments.展开更多
A variety of gold(Ⅲ) adducts having a-ligated oxygen-donor ligands have been prepared from [Au(ppy)Cl2](ppy.phenylpyridine)(1) either by partial or total replacement of the chloride ions. The new species comp...A variety of gold(Ⅲ) adducts having a-ligated oxygen-donor ligands have been prepared from [Au(ppy)Cl2](ppy.phenylpyridine)(1) either by partial or total replacement of the chloride ions. The new species comprise hydroxo-[Au(ppy)(OH)Cl](2), and [Au(ppy)(OH)2](3), oxo-[Au2(ppy)2(μ-O)2](4), acetate-[Au(ppy)(O2CMe2)] (5), and alkoxo complexes-[Au(ppy)(OR)Cl](6, 7) and [Au(ppy)(OR)2](8--10)(R=Me, 6 and 8; Et, 7 and 9; Pr, 10). The dihydroxo and the oxo complexes can be interconverted by refluxing the former in anhydrous THF and the latter in water. The hydroxides 2 and 3 and the acetato complex 5 undergo σ-ligand metathesis in ROH solution(R=Me, Et or Pr) to give the corresponding alkoxides.展开更多
o-Carboxybenzaldehyde (1)and acetone gave the Claisen-Schmidt condensation product, which readily cyclizes on acidification to give 1-oxo-3-acetonyl-dihydrobenzo [c]furan(4)in 68% yield. Other methyl ketones behaved s...o-Carboxybenzaldehyde (1)and acetone gave the Claisen-Schmidt condensation product, which readily cyclizes on acidification to give 1-oxo-3-acetonyl-dihydrobenzo [c]furan(4)in 68% yield. Other methyl ketones behaved similarly.展开更多
A series of some new 2-imino-5-[(Z)-1-(4-methylphenyl)methylidene]-3-[5-(2-oxo-2H-3-chromenyl)-1,3-oxazol-2-yl]-1,3- thiazolan-4-ones 5a-j has been synthesized and assayed for their antibacterial activity agains...A series of some new 2-imino-5-[(Z)-1-(4-methylphenyl)methylidene]-3-[5-(2-oxo-2H-3-chromenyl)-1,3-oxazol-2-yl]-1,3- thiazolan-4-ones 5a-j has been synthesized and assayed for their antibacterial activity against Gram-positive bacteria viz.Bacillus subtilis(ATCC 6633),Staphylococcus aureus(ATCC 6538p) and Micrococcus luteus(IFC 12708),and Gram-negative bacteria viz. Proteus vulgaris(ATCC 3851).Salmonella typhimurium(ATCC 14028) and Escherichia coli(ATCC 25922).Among the screened compounds,5d,5e,5f,5g,and 5j exhibited potent inhibitory activity compared to standard drug,and emerged as potential molecules for further development.展开更多
The effects of axial ligand on the oxygen atom transfer(OAT)reaction from 5,10,15-tris(pentafluorophenyl)corrole((tpfc)MnVO)to dimethyl sulfide(DMS)have been investigated by density functional theory(DFT)calculations....The effects of axial ligand on the oxygen atom transfer(OAT)reaction from 5,10,15-tris(pentafluorophenyl)corrole((tpfc)MnVO)to dimethyl sulfide(DMS)have been investigated by density functional theory(DFT)calculations.Imidazole(Im),4-methylimidazole(4-MI)and pyridine(Py)were selected as the axial ligands.The results revealed that the axial ligand can form coordinate bond with(tpfc)MnVO in the transition state(TS)of the OAT reaction.The axial coordination favored charge transferring from(tpfc)MnVO to DMS,and weakened the Mn≡O bond in both singlet and triplet states.Furthermore,axial coordination can reduce the energy barrier of neutral(tpfc)MnVO from 23.62 kJ·mol^-1 to less than 3 kJ·mol^-1 in the triplet state,which is significantly lower than in the singlet state.This makes(tpfc)MnVO tend to direct the OAT reaction via triplet state pathway.On the other hand,the energy barriers of[(tpfc)MnVIO]+species from disproportionation pathway increased from 1.26 to 33.95 kJ·mol^-1 in a doublet state.This suggests axial ligands were conducive for direct(tpfc)MnVO OAT reaction pathway.展开更多
The photocleavage abilities of a novel family of compounds, 8-oxo-8%H%-acenaphtho pyrrole-9-carbonitrile and its derivatives(compounds 1—5) were evaluated with M13 mp18 single strand circular DNA. Only compound 1 wit...The photocleavage abilities of a novel family of compounds, 8-oxo-8%H%-acenaphtho pyrrole-9-carbonitrile and its derivatives(compounds 1—5) were evaluated with M13 mp18 single strand circular DNA. Only compound 1 with a diethylamine group could bind to DNA %via% electrostatic attraction and intercalation. At a concentration of 50 μmol/L, it could generate singlet oxygen to cleave circular DNA into linear DNA under the irradiation of long wavelength light(λ>400 nm). The antitumor {ability} of compound 1 was also evaluated in vitro, and its IC_ 50 on HeLa cells was as low as 6.8 μmol/L.展开更多
The title compound N-tert-butyl-N(-(2,4-dichlorobenzoyl)-N-[1-(4-chlorophenyl)- 1,4-dihydro-6-methylpyridazine-4-oxo-3-carbonyl]hydrazine [(C23H_21N4O3Cl3)2·1.5H_2O, Mr = 1042.60] was prepared by the reaction of ...The title compound N-tert-butyl-N(-(2,4-dichlorobenzoyl)-N-[1-(4-chlorophenyl)- 1,4-dihydro-6-methylpyridazine-4-oxo-3-carbonyl]hydrazine [(C23H_21N4O3Cl3)2·1.5H_2O, Mr = 1042.60] was prepared by the reaction of 1-(4-chlorophenyl)-1,4-dihydro-4-oxo-6- methylpyridazine-3-carboxylic acid with chloroformate ethyl ester, then with N′-tert-butyl-N- (2,4-dichlorobenzoyl) hydrazine in the present of triethylamine. The crystal structure has been determined by X-ray diffraction. The crystal belongs to Monoclinic, space group P21/c, with unit cell constants a =11.4948(9), b=12.7495(10), c=35.854(3) ?, β =92.964(2)°, Z=4, V=5247.6(7) ?3, Dc = 1.320 Mg/m3, F(000) = 2156 , μ (MoKa)= 0.385, R = 0.0661, wR = 0.1875, for 9151 observed reflections( I >2σ(I)). The structure is a dimer linked by intermolecular hydrogen bond which can be observed between N(1)- H...O(6), N(5)- H...O(3). The distances are 2.068 and 2.027? respectively.展开更多
A sensitive and selective liquid chromatography-tandem mass spectrometric(LC —MS/MS)method was established to determine 2-oxo-clopidogrel,a crucial intermediate metabolite in human plasma.A chromatographic separati...A sensitive and selective liquid chromatography-tandem mass spectrometric(LC —MS/MS)method was established to determine 2-oxo-clopidogrel,a crucial intermediate metabolite in human plasma.A chromatographic separation was performed on a Sapphire C_(18) column following a liquid-liquid extraction sample preparation with methyl t-butyl ether.Detection was carried out on a triple quadrupole mass spectrometer operated in multiple reaction monitoring(MRM) with an electrospray ionization(ESI)mode.The method was validated in terms of specificity,accuracy,precision and limit of quantification.The calibration curves ranged from 0.50 to 50.0 ng/mL with good linearity.The stability was fully validated with addition of 1,4-dithio-DL-threitol(DTT) into the plasma sample prior to and in the preparation procedure.The validated method was proved to be suitable for use in pharmacokinetic study after single oral administration of 75 mg clopidogrel tablets in human subjects,which could make contribution to intensive study of the clinical drug-drug interactions of clopidogrel and individual treatment.展开更多
The crystal structure of the title compound ethyl 3-(4-chlorophenyl)-3,4-dihydro-6- methyl-4-oxo-2-(pyrrolidin-1-yl)furo[2,3-d]pyrimidine-5-carboxylate (C20H20ClN3O4, Mr= 401.84) has been prepared and determined...The crystal structure of the title compound ethyl 3-(4-chlorophenyl)-3,4-dihydro-6- methyl-4-oxo-2-(pyrrolidin-1-yl)furo[2,3-d]pyrimidine-5-carboxylate (C20H20ClN3O4, Mr= 401.84) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 20.6215(9), b = 8.5311(4), c = 21.6886(9) A^°, β = 91.607(1)°, V = 3814.0(3)A^°^3, Z = 8, Dc = 1.400 g/cm^3, F(000) = 1680, μ = 0.233 mm^-1, R = 0.0718 and wR = 0.1545 for 6717 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals two crystallographically independent molecules in the asymmetric unit.展开更多
The synthesis and structure of [Fe(Phen)3][(μ-oxo)Fe2Cl6]稤MF are reported. The crystal data for the compound: monoclinic, P2l /c,a =15.491(1),b = 13.217(1),c = 20.748(2)牛?= 93.83(3),V = 4239(2)?,Z = 4,Dc = 1.562g/c...The synthesis and structure of [Fe(Phen)3][(μ-oxo)Fe2Cl6]稤MF are reported. The crystal data for the compound: monoclinic, P2l /c,a =15.491(1),b = 13.217(1),c = 20.748(2)牛?= 93.83(3),V = 4239(2)?,Z = 4,Dc = 1.562g/cm3,μ(MoK)=1.44 mm-1,F(000)= 2040.0, (C39H31Cl6Fe3N7O2) and Mr = 1009.96. X-ray crystallographic studies reveal that the title compound contains complexes of [Fe(Phen)3]2+ and [Fe2(μ-oxo)Cl6]2- which consists of two [FeCl3] fragments connected by an oxo bridge,with the bond distances of Fe(3)O(1) 1.744(4) and Fe(2)O(1) 1.754(4)牛琣nd a bond angle Fe(2)O(1)Fe(3) of 162.9(3). In the [Fe2(μ-oxo)Cl6]2- complex, the two iron (Ⅲ) centres exhibit tetrahedral coordination, with the distorted tetrahedra formed by three Cl atoms and an oxo bridge. The bond lengths to the donor atoms lie in the range 2.211(1)~2.226(1)?for FeCl, and the non-bonded Fe…Fe distance is 3.459?展开更多
文摘目的探讨尿液中核酸氧化代谢产物8-oxo-Gsn和8-oxo-d Gsn对HBV感染引起肝损伤程度的评估价值。方法收集笔者医院94例慢性乙型肝炎(以下简称慢乙肝)患者行超声引导下肝穿刺活检前的尿液,95例健康者以及25例乙肝表面携带者的随机尿液,采用同位素稀释高效液相-串联质谱法(ID-LC-MS/MS)分析尿液中DNA氧化标志物8-oxod Gsn和RNA氧化标志物8-oxo-Gsn,并结合病理结果和生化指标(ALT和AST),分析各指标之间的相关性,通过ROC曲线评估二者对肝损伤程度的预测价值,并分析8-oxo-Gsn和8-oxo-d Gsn在不同炎症活动度和不同纤维化程度患者中的水平差异。结果实验组中,88.5%(46/52)的男性8-oxo-Gsn高于正常对照组,85.7%(36/42)的女性8-oxo-Gsn高于正常对照组;肝脏炎症程度高的患者(G_3~G_4)尿液中RNA氧化标志物8-oxo-Gsn显著高于炎症程度低的患者(G_0~G_2)(4.28 vs 3.26,χ~2=11.117,P=0.009),纤维化程度高的患者8-oxo-Gsn水平也高于纤维化程度低的患者(3.66 vs 3.29),但未达到显著性水平(χ~2=3.626,P=0.323)。尿液中RNA氧化标志物8-oxo-Gsn对肝脏炎症程度有较好的预测价值(敏感度为82.4%,特异性为75%,AUC=0.813),对纤维化程度有较好的预测价值(敏感度为83.3%,特异性为77.1%,AUC=0.824)。结论尿液中RNA氧化标志物8-oxo-Gsn可能是HBV感染引起的肝损伤严重程度的评估指标。
文摘目的探讨妊娠糖尿病(gestational diabetes mellitus,GDM)患者尿液RNA氧化标志物8G-氧化鸟苷(8-oxo-7,8-dihydroguanosine,8-oxo-Gsn)的水平及与妊娠结局的关系。方法选取2018年2月~2021年2月汉川市中医医院收治的106例GDM患者为观察组,根据妊娠结局情况分为妊娠结局良好组和妊娠结局不良组。另选取同期进行体检的90例健康孕妇为对照组。收集所有孕妇的临床资料并进行比较。采用同位素稀释高效液相-串联质谱法(isotope dilution high performance liquid phase-tandem mass spectrometry,ID-LC-MS/MS)分析尿液中8-oxo-Gsn水平。采用ROC曲线评估8-oxo-Gsn对GDM患者不良妊娠结局的评估价值。多因素回归分析影响GDM患者不良妊娠结局的危险因素。结果与对照组相比,观察组尿液8-oxo-Gsn水平(3.89±0.63μmol/mol vs 2.26±0.47μmol/mol)及不良妊娠结局的发生率(29.25%vs 11.11%)明显升高,差异有统计学意义(t=20.225,χ^(2)=9.676,均P<0.05)。与妊娠结局良好组相比,妊娠结局不良组患者尿液8-oxo-Gsn水平(4.67±0.77μmol/mol vs 3.56±0.57μmol/mol)升高,差异有统计学意义(t=8.197,P<0.05)。ROC曲线分析结果显示,8-oxo-Gsn预测GDM患者不良妊娠结局的曲线下面积为0.847,截断值为4.049μmol/mol,敏感度和特异度分别为77.40%,81.30%。HOMA-IR[OR(95%CI):4.726(2.027~11.021)],8-oxo-Gsn[OR(95%CI):5.591(2.239~13.964)]是GDM患者发生不良妊娠结局的独立危险因素(均P<0.05)。结论GDM患者尿液8-oxo-Gsn水平升高,与患者不良妊娠结局有关,且对不良妊娠结局具有较优的预测价值。
文摘The reaction mechanism of OXO(X=Cl, Br) with H(2\%S\%) was studied theoretically by using the B3LYP/6-311+G(3df, 3pd) and the high-level electron-correlation QCISD(T)/6-311+G ** at single-point. The results show that the mechanism for the title reaction involves three channels, from which OH+XO, HO 2+X and HX+O 2 products could be obtained, respectively. Therefore, the channel to yield the products OH+XO is the dominant one in agreement with the experiments.
基金Supported by the Ministerio De Ciencia Y Technologia(NoSB2004-oobo)
文摘A variety of gold(Ⅲ) adducts having a-ligated oxygen-donor ligands have been prepared from [Au(ppy)Cl2](ppy.phenylpyridine)(1) either by partial or total replacement of the chloride ions. The new species comprise hydroxo-[Au(ppy)(OH)Cl](2), and [Au(ppy)(OH)2](3), oxo-[Au2(ppy)2(μ-O)2](4), acetate-[Au(ppy)(O2CMe2)] (5), and alkoxo complexes-[Au(ppy)(OR)Cl](6, 7) and [Au(ppy)(OR)2](8--10)(R=Me, 6 and 8; Et, 7 and 9; Pr, 10). The dihydroxo and the oxo complexes can be interconverted by refluxing the former in anhydrous THF and the latter in water. The hydroxides 2 and 3 and the acetato complex 5 undergo σ-ligand metathesis in ROH solution(R=Me, Et or Pr) to give the corresponding alkoxides.
文摘o-Carboxybenzaldehyde (1)and acetone gave the Claisen-Schmidt condensation product, which readily cyclizes on acidification to give 1-oxo-3-acetonyl-dihydrobenzo [c]furan(4)in 68% yield. Other methyl ketones behaved similarly.
文摘A series of some new 2-imino-5-[(Z)-1-(4-methylphenyl)methylidene]-3-[5-(2-oxo-2H-3-chromenyl)-1,3-oxazol-2-yl]-1,3- thiazolan-4-ones 5a-j has been synthesized and assayed for their antibacterial activity against Gram-positive bacteria viz.Bacillus subtilis(ATCC 6633),Staphylococcus aureus(ATCC 6538p) and Micrococcus luteus(IFC 12708),and Gram-negative bacteria viz. Proteus vulgaris(ATCC 3851).Salmonella typhimurium(ATCC 14028) and Escherichia coli(ATCC 25922).Among the screened compounds,5d,5e,5f,5g,and 5j exhibited potent inhibitory activity compared to standard drug,and emerged as potential molecules for further development.
基金supported by the National Natural Science Foundation of China(21275057,21671068)Natural Science Foundation of Guangdong Province(S2012010008763,2017A050506048)
文摘The effects of axial ligand on the oxygen atom transfer(OAT)reaction from 5,10,15-tris(pentafluorophenyl)corrole((tpfc)MnVO)to dimethyl sulfide(DMS)have been investigated by density functional theory(DFT)calculations.Imidazole(Im),4-methylimidazole(4-MI)and pyridine(Py)were selected as the axial ligands.The results revealed that the axial ligand can form coordinate bond with(tpfc)MnVO in the transition state(TS)of the OAT reaction.The axial coordination favored charge transferring from(tpfc)MnVO to DMS,and weakened the Mn≡O bond in both singlet and triplet states.Furthermore,axial coordination can reduce the energy barrier of neutral(tpfc)MnVO from 23.62 kJ·mol^-1 to less than 3 kJ·mol^-1 in the triplet state,which is significantly lower than in the singlet state.This makes(tpfc)MnVO tend to direct the OAT reaction via triplet state pathway.On the other hand,the energy barriers of[(tpfc)MnVIO]+species from disproportionation pathway increased from 1.26 to 33.95 kJ·mol^-1 in a doublet state.This suggests axial ligands were conducive for direct(tpfc)MnVO OAT reaction pathway.
文摘The photocleavage abilities of a novel family of compounds, 8-oxo-8%H%-acenaphtho pyrrole-9-carbonitrile and its derivatives(compounds 1—5) were evaluated with M13 mp18 single strand circular DNA. Only compound 1 with a diethylamine group could bind to DNA %via% electrostatic attraction and intercalation. At a concentration of 50 μmol/L, it could generate singlet oxygen to cleave circular DNA into linear DNA under the irradiation of long wavelength light(λ>400 nm). The antitumor {ability} of compound 1 was also evaluated in vitro, and its IC_ 50 on HeLa cells was as low as 6.8 μmol/L.
文摘The title compound N-tert-butyl-N(-(2,4-dichlorobenzoyl)-N-[1-(4-chlorophenyl)- 1,4-dihydro-6-methylpyridazine-4-oxo-3-carbonyl]hydrazine [(C23H_21N4O3Cl3)2·1.5H_2O, Mr = 1042.60] was prepared by the reaction of 1-(4-chlorophenyl)-1,4-dihydro-4-oxo-6- methylpyridazine-3-carboxylic acid with chloroformate ethyl ester, then with N′-tert-butyl-N- (2,4-dichlorobenzoyl) hydrazine in the present of triethylamine. The crystal structure has been determined by X-ray diffraction. The crystal belongs to Monoclinic, space group P21/c, with unit cell constants a =11.4948(9), b=12.7495(10), c=35.854(3) ?, β =92.964(2)°, Z=4, V=5247.6(7) ?3, Dc = 1.320 Mg/m3, F(000) = 2156 , μ (MoKa)= 0.385, R = 0.0661, wR = 0.1875, for 9151 observed reflections( I >2σ(I)). The structure is a dimer linked by intermolecular hydrogen bond which can be observed between N(1)- H...O(6), N(5)- H...O(3). The distances are 2.068 and 2.027? respectively.
文摘A sensitive and selective liquid chromatography-tandem mass spectrometric(LC —MS/MS)method was established to determine 2-oxo-clopidogrel,a crucial intermediate metabolite in human plasma.A chromatographic separation was performed on a Sapphire C_(18) column following a liquid-liquid extraction sample preparation with methyl t-butyl ether.Detection was carried out on a triple quadrupole mass spectrometer operated in multiple reaction monitoring(MRM) with an electrospray ionization(ESI)mode.The method was validated in terms of specificity,accuracy,precision and limit of quantification.The calibration curves ranged from 0.50 to 50.0 ng/mL with good linearity.The stability was fully validated with addition of 1,4-dithio-DL-threitol(DTT) into the plasma sample prior to and in the preparation procedure.The validated method was proved to be suitable for use in pharmacokinetic study after single oral administration of 75 mg clopidogrel tablets in human subjects,which could make contribution to intensive study of the clinical drug-drug interactions of clopidogrel and individual treatment.
基金supported by the Natural Science Foundation of Hubei Province (2006ABB016)Key Science Research Project of Hubei Provincial Department of Education (No.D200724001) the Science Research Project of Yunyang Medical College (No. 2006QDJ16)
文摘The crystal structure of the title compound ethyl 3-(4-chlorophenyl)-3,4-dihydro-6- methyl-4-oxo-2-(pyrrolidin-1-yl)furo[2,3-d]pyrimidine-5-carboxylate (C20H20ClN3O4, Mr= 401.84) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 20.6215(9), b = 8.5311(4), c = 21.6886(9) A^°, β = 91.607(1)°, V = 3814.0(3)A^°^3, Z = 8, Dc = 1.400 g/cm^3, F(000) = 1680, μ = 0.233 mm^-1, R = 0.0718 and wR = 0.1545 for 6717 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals two crystallographically independent molecules in the asymmetric unit.
基金Supported by the foundation of Education Committee of Fujian Province (JB01045)
文摘The synthesis and structure of [Fe(Phen)3][(μ-oxo)Fe2Cl6]稤MF are reported. The crystal data for the compound: monoclinic, P2l /c,a =15.491(1),b = 13.217(1),c = 20.748(2)牛?= 93.83(3),V = 4239(2)?,Z = 4,Dc = 1.562g/cm3,μ(MoK)=1.44 mm-1,F(000)= 2040.0, (C39H31Cl6Fe3N7O2) and Mr = 1009.96. X-ray crystallographic studies reveal that the title compound contains complexes of [Fe(Phen)3]2+ and [Fe2(μ-oxo)Cl6]2- which consists of two [FeCl3] fragments connected by an oxo bridge,with the bond distances of Fe(3)O(1) 1.744(4) and Fe(2)O(1) 1.754(4)牛琣nd a bond angle Fe(2)O(1)Fe(3) of 162.9(3). In the [Fe2(μ-oxo)Cl6]2- complex, the two iron (Ⅲ) centres exhibit tetrahedral coordination, with the distorted tetrahedra formed by three Cl atoms and an oxo bridge. The bond lengths to the donor atoms lie in the range 2.211(1)~2.226(1)?for FeCl, and the non-bonded Fe…Fe distance is 3.459?