In order to prepare a high capacity packing material for solid-phase extraction with specific recognition ability of trace ractopamine in biological samples, uniformly-sized, molecularly imprinted polymers (MIPs) were prepared by a multi-step swelling and polymerization method using methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, and toluene as a porogen respectively. Scanning electron microscope and specific surface area were employed to identify the characteristics of MIPs. Ultraviolet spectroscopy, Fourier transform infrared spectroscopy, Scatchard analysis and kinetic study were performed to interpret the specific recognition ability and the binding process of MIPs. The results showed that, compared with other reports, MIPs synthetized in this study showed high adsorption capacity besides specific recognition ability. The adsorption capacity of MIPs was 0.063 mmol/g at 1 mmol/L ractopamine concentration with the distribution coefficient 1.70. The resulting MIPs could be used as solid-phase extraction materials for separation and enrichment of trace ractopamine in biological samples.
Ya LiQiang FuMeng LiuYuan-Yuan JiaoWei DuChong YuJing LiuChun ChangJian Lu
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 μg/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 ampicillin 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.
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.
Aiguo ZengXia LiuSiruo ZhangYan ZhengPing HuangKangli DuQiang Fu
