目的:建立柱后衍生化高效液相色谱法测定硫酸阿米卡星含量的方法。方法:色谱柱为Waters Sun Fire C18(4.6mm×150mm,5μm);流动相为含戊烷磺酸钠和冰醋酸的硫酸钠溶液-甲醇(97∶3);柱温25℃,流速1.0mL.min-1。柱后衍生化试液为邻苯...目的:建立柱后衍生化高效液相色谱法测定硫酸阿米卡星含量的方法。方法:色谱柱为Waters Sun Fire C18(4.6mm×150mm,5μm);流动相为含戊烷磺酸钠和冰醋酸的硫酸钠溶液-甲醇(97∶3);柱温25℃,流速1.0mL.min-1。柱后衍生化试液为邻苯二甲醛溶液,流速0.5mL·min-1,衍生化反应温度45℃,荧光激发波长360nm,测定波长440nm。结果:硫酸阿米卡星在2.09～41.81mg·L-1浓度范围内线性关系良好(r=0.9999),平均回收率(n=9)为98.6%。结论:该方法简便快速,结果准确可靠,可用于注射用硫酸阿米卡星的含量测定。展开更多
CdTe nanocrystals(CdTe NCs) were achieved by reaction of CdCl2 with KHTe solution and were capped with sodium mercaptoacetate.The product was detected by transmission electron microscopy(TEM),high-resolution transmiss...CdTe nanocrystals(CdTe NCs) were achieved by reaction of CdCl2 with KHTe solution and were capped with sodium mercaptoacetate.The product was detected by transmission electron microscopy(TEM),high-resolution transmission electron microscopy(HRTEM),energy dispersive spectroscopy(EDS),fluorescence spectra,ultraviolet-visible spectra and X-ray diffraction(XRD).The CdTe NCs are of cubic structure and the average size is about 5 nm.The fluorescence quantum yield of CdTe NCs aqueous solution increased from 37% to 97% after 20 d under room light.The maximum λem of fluorescence changed from 543 nm to 510 nm and the blue shift was 33 nm.CdTe NCs aqueous solution can be steady for at least 10 months at 4℃ in a refrigerator.The resonance Rayleigh scattering(RRS) of CdTe NCs in the aqueous solution was investigated.The maximum scattering peak was located at about 554 nm.The interactions of CdTe NCs with amikacin sulfate(AS) and micronomicin sulfate(MS) were investigated respectively.The effects of AS and MS on fluorescence and RRS of CdTe NCs were analyzed.It was found that AS and MS quenched the photoluminescence of CdTe NCs and enhanced RRS of CdTe NCs.Under optimum conditions,there are linear relationships between quenching intensity(F0-F),intensity of RRS(I-I0) and concentration of AS and MS.The detection limits(3б) of AS and MS are respectively 3.4 ng·mL-1 and 2.6 ng·mL-1 by the fluorescence quenching method,and 15.2 ng·mL-1 and 14.0 ng·mL-1 by the RRS method.The methods have high sensitivity,thus CdTe NCs may be used as fluorescence probes and RRS probes for the detection of aminoglycoside antibiotics.展开更多
文摘目的:建立柱后衍生化高效液相色谱法测定硫酸阿米卡星含量的方法。方法:色谱柱为Waters Sun Fire C18(4.6mm×150mm,5μm);流动相为含戊烷磺酸钠和冰醋酸的硫酸钠溶液-甲醇(97∶3);柱温25℃,流速1.0mL.min-1。柱后衍生化试液为邻苯二甲醛溶液,流速0.5mL·min-1,衍生化反应温度45℃,荧光激发波长360nm,测定波长440nm。结果:硫酸阿米卡星在2.09～41.81mg·L-1浓度范围内线性关系良好(r=0.9999),平均回收率(n=9)为98.6%。结论:该方法简便快速,结果准确可靠,可用于注射用硫酸阿米卡星的含量测定。
基金Supported by the National Natural Science Foundation of China (Grant No. 20475045)
文摘CdTe nanocrystals(CdTe NCs) were achieved by reaction of CdCl2 with KHTe solution and were capped with sodium mercaptoacetate.The product was detected by transmission electron microscopy(TEM),high-resolution transmission electron microscopy(HRTEM),energy dispersive spectroscopy(EDS),fluorescence spectra,ultraviolet-visible spectra and X-ray diffraction(XRD).The CdTe NCs are of cubic structure and the average size is about 5 nm.The fluorescence quantum yield of CdTe NCs aqueous solution increased from 37% to 97% after 20 d under room light.The maximum λem of fluorescence changed from 543 nm to 510 nm and the blue shift was 33 nm.CdTe NCs aqueous solution can be steady for at least 10 months at 4℃ in a refrigerator.The resonance Rayleigh scattering(RRS) of CdTe NCs in the aqueous solution was investigated.The maximum scattering peak was located at about 554 nm.The interactions of CdTe NCs with amikacin sulfate(AS) and micronomicin sulfate(MS) were investigated respectively.The effects of AS and MS on fluorescence and RRS of CdTe NCs were analyzed.It was found that AS and MS quenched the photoluminescence of CdTe NCs and enhanced RRS of CdTe NCs.Under optimum conditions,there are linear relationships between quenching intensity(F0-F),intensity of RRS(I-I0) and concentration of AS and MS.The detection limits(3б) of AS and MS are respectively 3.4 ng·mL-1 and 2.6 ng·mL-1 by the fluorescence quenching method,and 15.2 ng·mL-1 and 14.0 ng·mL-1 by the RRS method.The methods have high sensitivity,thus CdTe NCs may be used as fluorescence probes and RRS probes for the detection of aminoglycoside antibiotics.
