A simple and sensitive liquid chromatographic method was developed for quantification of cefotetan disodium (CTT),a semi-synthetic cephamycin antibiotic,in human plasma.CTT and the internal standard chloramphenicol we...A simple and sensitive liquid chromatographic method was developed for quantification of cefotetan disodium (CTT),a semi-synthetic cephamycin antibiotic,in human plasma.CTT and the internal standard chloramphenicol were extracted from plasma by a simple one-step protein precipitation with 35% (v/v) perchloric acid.Separation was carried out on a reverse-phase C18 column with a mobile phase of acetonitile-water containing 0.5% (v/v) phosphoric acids (20:80,v/v) at a flow rate of 1.0 mL/min.The column effluent was monitored by UV detection at 300 nm.The column temperature was maintained at 40°C.This method demonstrated good linearity in the range of 0.525-300.0 μg/mL,with correlation coefficients greater than 0.99.The limit of quantification (LOQ) was 0.525 μg/mL in human plasma.Intra-and inter-day precisions were less than 6.63% in terms of relative standard deviation (RSD).The accuracy,when expressed by the bias,ranged from 0.57% to 4.04%.The mean extraction recovery of CTT was higher than 40.94%.The method was found to be precise,accurate,and specific for CTT quantitative analysis,and was successfully applied for a pharmacokinetic study of CTT after a single intravenous dose of 1.0 g of CTT in healthy Chinese subjects.展开更多
A rapid and sensitive liquid chromatography-tandem mass spectrometry（LC-MS/MS） method for the de- termination of cefotetan in human plasma was developed and validated. After the protein precipitation of sample with ...A rapid and sensitive liquid chromatography-tandem mass spectrometry（LC-MS/MS） method for the de- termination of cefotetan in human plasma was developed and validated. After the protein precipitation of sample with acetonitrile, the analyte and internal standard（IS）, tramadol, were separated on a Zorbax XDB C8 column using ace- tonitrile/1%（volume fraction） formic acid（volume ratio 35：65, pH=2.5） as mobile phase at a flow rate of 1.0 mL/min with a 1 ： 1 split. The detection was performed by electrospray ionization with positive ion mode, followed by multiple reaction monitoring of the transitions for cefotetan at m/z 576.3→460.2（quantifier） and m/z 576.3→432.2（qualifier） and for IS at m/z 264.1→58.1. Cefotetan and IS were eluted at 1.86 and 1.87 rain, respectively. The assay was linear over the concentration range of 0.1-100 gg/mL for 20 μL of human plasma only with intra- and inter-day preci- sions（expressed as the relative standard deviation） of less than 6.62% and accuracies（as relative error） of ＋1.31%. The method was applied to the pharmacokinetic study of a l-h intravenous infusion of 1.0 g of cefotetan disodium for human volunteers（n=6）.展开更多
基金supported by a grant of the Guangzhou Boji Clinical Research Center of New Drugs,Guangzhou,Guangdong,China
文摘A simple and sensitive liquid chromatographic method was developed for quantification of cefotetan disodium (CTT),a semi-synthetic cephamycin antibiotic,in human plasma.CTT and the internal standard chloramphenicol were extracted from plasma by a simple one-step protein precipitation with 35% (v/v) perchloric acid.Separation was carried out on a reverse-phase C18 column with a mobile phase of acetonitile-water containing 0.5% (v/v) phosphoric acids (20:80,v/v) at a flow rate of 1.0 mL/min.The column effluent was monitored by UV detection at 300 nm.The column temperature was maintained at 40°C.This method demonstrated good linearity in the range of 0.525-300.0 μg/mL,with correlation coefficients greater than 0.99.The limit of quantification (LOQ) was 0.525 μg/mL in human plasma.Intra-and inter-day precisions were less than 6.63% in terms of relative standard deviation (RSD).The accuracy,when expressed by the bias,ranged from 0.57% to 4.04%.The mean extraction recovery of CTT was higher than 40.94%.The method was found to be precise,accurate,and specific for CTT quantitative analysis,and was successfully applied for a pharmacokinetic study of CTT after a single intravenous dose of 1.0 g of CTT in healthy Chinese subjects.
基金Supported by the National Natural Science Foundation of China（Nos.81430087, 81473142, 81102383） and the Prej ect of China Equipment and Education Resources System（CERS）（No.CERS-1-70）.
文摘A rapid and sensitive liquid chromatography-tandem mass spectrometry（LC-MS/MS） method for the de- termination of cefotetan in human plasma was developed and validated. After the protein precipitation of sample with acetonitrile, the analyte and internal standard（IS）, tramadol, were separated on a Zorbax XDB C8 column using ace- tonitrile/1%（volume fraction） formic acid（volume ratio 35：65, pH=2.5） as mobile phase at a flow rate of 1.0 mL/min with a 1 ： 1 split. The detection was performed by electrospray ionization with positive ion mode, followed by multiple reaction monitoring of the transitions for cefotetan at m/z 576.3→460.2（quantifier） and m/z 576.3→432.2（qualifier） and for IS at m/z 264.1→58.1. Cefotetan and IS were eluted at 1.86 and 1.87 rain, respectively. The assay was linear over the concentration range of 0.1-100 gg/mL for 20 μL of human plasma only with intra- and inter-day preci- sions（expressed as the relative standard deviation） of less than 6.62% and accuracies（as relative error） of ＋1.31%. The method was applied to the pharmacokinetic study of a l-h intravenous infusion of 1.0 g of cefotetan disodium for human volunteers（n=6）.
