Surface molecularly imprinted polymers （SMIPs） for selective adsorption of ampicillin sodium were synthesized using surface molecular imprinting technique with silica gel as a support. The physical and morphological...Surface molecularly imprinted polymers （SMIPs） for selective adsorption of ampicillin sodium were synthesized using surface molecular imprinting technique with silica gel as a support. The physical and morphological characteristics of the polymers were investigated by scanning electron microscope （SEM）, Fourier transform infrared spectroscopy （FT-IR）, thermogravimetric analysis （TGA）, elemental analysis and nitrogen adsorption-desorption test. The obtained results showed that the SMIPs displayed great adsorption capacity （13.5 lag/mg）, high recognition ability （the imprinted factor is 3.2） and good binding kinetics for ampicillin sodium. Finally, as solid phase extraction adsorbents, the SMIPs coupled with HPLC method were validated and applied for the enrichment, purification and determination of anapicillin sodium in real milk and blood samples. The averages of spiked accuracy ranged from 92.1% to 107.6%. The relative standard deviations of intra- and inter-day precisions were less than 4.6%. This study provides a new and promising method for enriching, extracting and determining ampicillin sodium in complex biological samples.展开更多
A simple high-performance liquid chromatography(HPLC)method coupled with an evaporative light scattering detector(ELSD)was developed for the determination of azithromycin in raw materials and pharmaceutical formulatio...A simple high-performance liquid chromatography(HPLC)method coupled with an evaporative light scattering detector(ELSD)was developed for the determination of azithromycin in raw materials and pharmaceutical formulations(injections,capsules and tablets)without any pretreatment or derivatization step.Azithromycin,degradation products and formulation ingredients were separated efficiently by using the mobile phase consisted of ammonium acetate(0.05 M,pH 8.0)and acetonitrile(60:40,v/v)in an isocratic mode at 0.8 ml/min flow rate.Parameters of ELSD were 60C for evaporation temperature and 50 psi for pressure of carrier gas(air).A logarithmic calibration curve was obtained from 50.93 to 509.30 mg/ml(r¼0.9996)for azithromycin,with the limit of detection(LOD)of 6.75 mg/ml(S/n¼3)and the limit of quantification of 22.50 mg/ml(S/n¼10).The developed method was validated and applied with satisfactory accuracy and precision for the determination of azithromycin in raw materials and pharmaceutical formulations(recovery 99e102%,RSD<1.2%,n¼3).No significant difference(t-test)was found between the results of the developed HPLCeELSD method and the HPLCeUV or microbiological method.展开更多
基金financially supported by the National Natural Science Foundation of China (Nos. 81573391 and 81173024)the National Key Projects of China (No. 812277802)
文摘Surface molecularly imprinted polymers （SMIPs） for selective adsorption of ampicillin sodium were synthesized using surface molecular imprinting technique with silica gel as a support. The physical and morphological characteristics of the polymers were investigated by scanning electron microscope （SEM）, Fourier transform infrared spectroscopy （FT-IR）, thermogravimetric analysis （TGA）, elemental analysis and nitrogen adsorption-desorption test. The obtained results showed that the SMIPs displayed great adsorption capacity （13.5 lag/mg）, high recognition ability （the imprinted factor is 3.2） and good binding kinetics for ampicillin sodium. Finally, as solid phase extraction adsorbents, the SMIPs coupled with HPLC method were validated and applied for the enrichment, purification and determination of anapicillin sodium in real milk and blood samples. The averages of spiked accuracy ranged from 92.1% to 107.6%. The relative standard deviations of intra- and inter-day precisions were less than 4.6%. This study provides a new and promising method for enriching, extracting and determining ampicillin sodium in complex biological samples.
基金National Natural Science Foundations of China(No.81173024)to professor Qiang Fu is gratefully acknowledged.The authors also thank Xi’an Insti-tute of Food and Drug Control for providing the facilities and necessary equipments.
文摘A simple high-performance liquid chromatography(HPLC)method coupled with an evaporative light scattering detector(ELSD)was developed for the determination of azithromycin in raw materials and pharmaceutical formulations(injections,capsules and tablets)without any pretreatment or derivatization step.Azithromycin,degradation products and formulation ingredients were separated efficiently by using the mobile phase consisted of ammonium acetate(0.05 M,pH 8.0)and acetonitrile(60:40,v/v)in an isocratic mode at 0.8 ml/min flow rate.Parameters of ELSD were 60C for evaporation temperature and 50 psi for pressure of carrier gas(air).A logarithmic calibration curve was obtained from 50.93 to 509.30 mg/ml(r¼0.9996)for azithromycin,with the limit of detection(LOD)of 6.75 mg/ml(S/n¼3)and the limit of quantification of 22.50 mg/ml(S/n¼10).The developed method was validated and applied with satisfactory accuracy and precision for the determination of azithromycin in raw materials and pharmaceutical formulations(recovery 99e102%,RSD<1.2%,n¼3).No significant difference(t-test)was found between the results of the developed HPLCeELSD method and the HPLCeUV or microbiological method.
