摘要
目的建立反相高效液相色谱法（RP-HPLC）测定人血浆及尿中头孢唑兰浓度。方法采用Welch Materials XB C18（4.6mm×150 mm,5μm）色谱柱,血样及尿样流动相分别为乙腈-0.01 mol.L-1醋酸钠-三乙胺（6∶94∶0.001,醋酸调pH为3.52）和乙腈-0.01 mol.L-1醋酸钠-三乙胺（3∶97∶0.001,醋酸调pH为3.55）,检测波长为235 nm。血浆样品加乙腈沉淀蛋白后再用二氯甲烷反复洗后进样,内标为氟苷。尿样用纯水直接稀释后进样,外标法定量。结果血浆样品标准曲线在0.15~307.2 mg.L-1范围内线性关系良好,最低定量浓度为0.15 mg.L-1,预处理回收率为86.9%~108.4%,批内及批间RSD分别小于2.4%和5.4%。尿样标准曲线在4.69~4 800 mg.L-1内线性关系良好,最低定量浓度为4.69 mg.L-1,批内及批间RSD分别小于3.0%和5.9%。结论本法具有快速简便,灵敏准确等特点,适用于血浆及尿中头孢唑兰浓度测定。
OBJECTIVE To establish a RP-HPLC method for the determination of cefozopran in human plasma and urine.METHODS The assay was conducted on a HPLC-UV system consisted of a Welch Materials XB C18 column（4.6 mm×150 mm,5 μm）.The mobile phase for plasma and urine were acetonitrile-0.01 mol·L-1 sodium acetate-triethylamine（6∶94∶0.001,pH adjusted to 3.52 with acetic acid） and acetonitrile-0.01 mol·L-1 sodium acetate-triethylamine（3∶97∶0.001,pH adjusted to 3.55 with acetic acid）,respectively.Detection was performed at 235 nm.Plasma sample was first treated with acetonitrile for precipitation of proteins.The supernatant was then back washed by dichloromethane.The internal standard was Floxuridine.Urine was simply diluted with purified water and quantified by external reference method.RESULTS For plasma,the calibration curve was linear in the range from 0.15 to 307.2 mg·L-1,the limit of quantitation was 0.15 mg·L-1,the recovery of pretreatment was 86.9%-108.4%,the inter-and intra-day RSDs were less than 2.4% and 5.4%,respectively.For urine,the calibration curve was linear in the range from 4.69 to 4 800 mg·L-1,the limit of quantitation was 4.69 mg·L-1,the inter-and intra-day RSDs were less than 3.0% and 5.9%,respectively.CONCLUSION The methods is simple,rapid,sensitive and accurate for the determination of cefozopran in human plasma and urine.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2011年第7期545-548,共4页
Chinese Pharmaceutical Journal
