Two U0^(2+)_(2) complexes{[C_(5)H_(4)N(0)C=N-N=C(PhHPh)C=N-N=C(0)-C_(5)H_(4)N]2U02(CH30H)}(I)and{[C_(5)H_(4)N(0)ON-N=C(Ph)-(Ph)C=N-N=C(0)-C_(5)H_(4)N]2U02(C_(5)H_(4)N(0)C=N-NH_(2))}(II)were synthesized and characteriz...Two U0^(2+)_(2) complexes{[C_(5)H_(4)N(0)C=N-N=C(PhHPh)C=N-N=C(0)-C_(5)H_(4)N]2U02(CH30H)}(I)and{[C_(5)H_(4)N(0)ON-N=C(Ph)-(Ph)C=N-N=C(0)-C_(5)H_(4)N]2U02(C_(5)H_(4)N(0)C=N-NH_(2))}(II)were synthesized and characterized by IR,elemental analysis and thermal stability analysis,and the crystal structures were determined by X-ray diffraction.The crystal of complex I belongs to monoclinic system,space group P2_(1/n) with α=11.7678(4),6=16.9667(6),c=14.3051(5)A,β=98.918(3)°,Z=4,F=2821.64(17)A^(3),D_(c)=1.837 Mg·m^(-3),μ(MoKα)=5.805 mm^(-1),F(000)=1504,R=0.0346 and wR=0.0688.The crystal of complex II is of triclinic system,space group Pi with a=11.6417(5),b=11.7297(5),c=14.2197(5)A,α=71.697(4)°,β=86.020(3)°,γ=71.572(4)°,Z=2,K=1748.02(12)A^(3),D_(c)=1.742 Mg·m^(-3),μ(MoKa)=4.704 mm^(-1),F(000)=894,R=0.0283 and wR=0.0537.The U1 is a seven-coordinate pentagonal bipyramidal configuration in I and an eight-coordinate hexagonal dipyramidal configuration in II.The thermal stability and quantum chemical calculations of I and II were also investigated.展开更多
A sensitive and selective method employing chemiluminescence(CL)coupled with flow injection(FI)is reported for nalbuphine hydrochloride(NAL)assay in pharmaceutical formulations.The enhancement effect of NAL on the CL ...A sensitive and selective method employing chemiluminescence(CL)coupled with flow injection(FI)is reported for nalbuphine hydrochloride(NAL)assay in pharmaceutical formulations.The enhancement effect of NAL on the CL reaction between tris(2,2′-bipyridyl)ruthenium(II)chloride-diperiodatocuprate(III){Ru[(bpy)_(3)]^(2+)-Cu(III)complex}in acidic medium is used as analytical measurement.The optimal conditions of the CL reaction were sulfuric acid 1.0×10^(−3) mol/L,Ru[(bpy)s]2+7.5×10^(−5) mol/L,Cu(III)/Ag(III)complexes 4.0×10^(−4)/5.0×10^(−4) mol/L,sample loop volume of 120µL and flow rate of 2.5 mL/min.The sensitivities of the method in terms of detection(S/N=3)and quantification(S/N=10)limits are 5×10^(−4) and 0.001 ppm(1 ppm=1 mg/L),respectively.The linear response of the instrument in the form of CL intensity with respect to NAL concentration is over the range 0.001-15.0 ppm(R^(2)=0.9999)with relative standard deviation from 0.8%to 3.2%and injection throughput of 120 injection/h.The applications of the method include the quantitative analysis of NAL in pharmaceutical injection samples.Variations and the average results of the proposed method are not significantly different from the results of a reported method by applying F-and paired student t-test.The most likely CL reaction mechanism is written in accordance with spectrophotometric and CL studies.展开更多
基金Supported by the Foundation of Hunan Provincial Engineering Research Center for Uranium Exploration Technology(No.YK20K03)。
文摘Two U0^(2+)_(2) complexes{[C_(5)H_(4)N(0)C=N-N=C(PhHPh)C=N-N=C(0)-C_(5)H_(4)N]2U02(CH30H)}(I)and{[C_(5)H_(4)N(0)ON-N=C(Ph)-(Ph)C=N-N=C(0)-C_(5)H_(4)N]2U02(C_(5)H_(4)N(0)C=N-NH_(2))}(II)were synthesized and characterized by IR,elemental analysis and thermal stability analysis,and the crystal structures were determined by X-ray diffraction.The crystal of complex I belongs to monoclinic system,space group P2_(1/n) with α=11.7678(4),6=16.9667(6),c=14.3051(5)A,β=98.918(3)°,Z=4,F=2821.64(17)A^(3),D_(c)=1.837 Mg·m^(-3),μ(MoKα)=5.805 mm^(-1),F(000)=1504,R=0.0346 and wR=0.0688.The crystal of complex II is of triclinic system,space group Pi with a=11.6417(5),b=11.7297(5),c=14.2197(5)A,α=71.697(4)°,β=86.020(3)°,γ=71.572(4)°,Z=2,K=1748.02(12)A^(3),D_(c)=1.742 Mg·m^(-3),μ(MoKa)=4.704 mm^(-1),F(000)=894,R=0.0283 and wR=0.0537.The U1 is a seven-coordinate pentagonal bipyramidal configuration in I and an eight-coordinate hexagonal dipyramidal configuration in II.The thermal stability and quantum chemical calculations of I and II were also investigated.
文摘A sensitive and selective method employing chemiluminescence(CL)coupled with flow injection(FI)is reported for nalbuphine hydrochloride(NAL)assay in pharmaceutical formulations.The enhancement effect of NAL on the CL reaction between tris(2,2′-bipyridyl)ruthenium(II)chloride-diperiodatocuprate(III){Ru[(bpy)_(3)]^(2+)-Cu(III)complex}in acidic medium is used as analytical measurement.The optimal conditions of the CL reaction were sulfuric acid 1.0×10^(−3) mol/L,Ru[(bpy)s]2+7.5×10^(−5) mol/L,Cu(III)/Ag(III)complexes 4.0×10^(−4)/5.0×10^(−4) mol/L,sample loop volume of 120µL and flow rate of 2.5 mL/min.The sensitivities of the method in terms of detection(S/N=3)and quantification(S/N=10)limits are 5×10^(−4) and 0.001 ppm(1 ppm=1 mg/L),respectively.The linear response of the instrument in the form of CL intensity with respect to NAL concentration is over the range 0.001-15.0 ppm(R^(2)=0.9999)with relative standard deviation from 0.8%to 3.2%and injection throughput of 120 injection/h.The applications of the method include the quantitative analysis of NAL in pharmaceutical injection samples.Variations and the average results of the proposed method are not significantly different from the results of a reported method by applying F-and paired student t-test.The most likely CL reaction mechanism is written in accordance with spectrophotometric and CL studies.
