摘要
目的建立HPLC－uV法测定人血浆及尿中头孢他美钠的浓度。方法采用UltimateXB．C18（150×4．6mm，5um）色谱柱，血浆及尿样测定用流动相分别为20mmol／L醋酸铵：乙腈（90：10，V／V，醋酸调pH为5．08）和10mmol／L甲酸铵：乙腈（90：10，V／V，甲酸调pH为3．53），流速均为lmL／min，检测波长为265nm。血浆样品经乙腈沉淀蛋白，再用二氯甲烷反洗后取上清液进样，以头孢唑肟钠做内标，按内标法定量；尿样用纯水直接稀释后进样，外标法定量。结果血药浓度在0．125～320gg／mL范围内与峰面积线性关系良好，最低定量浓度为0．125ug／mL；预处理回收率为98．6％～105．9％：批内及批间精密度RSD分别小于2．0％和2．1％。尿药浓度在2～2000gg／mL范围内与峰面积线性关系良好，最低定量浓度为2ug／mL；批内及批问精密度RSD分别小于3．4％和4．1％。结论本法具有简便、灵敏、准确等特点，适用于人血浆及尿中头孢他美钠浓度的测定。
To establish a HPLC-UV method for the determination of cefetamet sodium in human plasma and urine. Methods The assay was conducted on a HPLC-UV system consisted of Ultimate XB-Ct8（150× 4.6ram, 5um）. The mobile phase were acetonitrile-20mmol/L ammonium acetate（90：10, V/V, pH was adjusted to 5.08 with acetate acid） and acetonitrile-10mmol/L ammonium formate（90：10, V/V, pH was adjusted to 3.53 with formate acid）, respectively. The mobile phase was pumped at 1 mL/min through the colum. The detection wavelengths was set at 265nm. Plasma sample was first deproteinization by acetonitrile, followed by extraction and removal of the acetonitrile with 2.5mL methylene chloride, Ceftizoxime sodium was used as internal standard（IS）. Urine sample was diluted by distilled water and quantified by external reference method. Result For plasma, the calibration curve was linear in the range from 0.125 to 320~tg/mL, the lowest limit of quantization was 0.125ug/mL. The recovery of plasma pretreatment was 98.6%-105.9%; the intra-day and inter-day RSD were less than 2.0% and 2.1%, respectively. For Urine, the calibration curve was linear in the range from 2 to 2000ug/mL, the lowest limit of quantization was 2ug/mL. The intra-day and inter-day RSD were less than 3.4% and 4.1%, respectively. Conclusion The methods is simple, rapid, sensitive and accurate for the determination of cefetamet sodium in human plasma and urine.
出处
《中国抗生素杂志》
CAS
CSCD
北大核心
2013年第10期756-759,共4页
Chinese Journal of Antibiotics
