摘要
[目的]采用HPLC/UV法检测家兔血浆中克林霉素。[方法]血清样品经乙腈沉淀蛋白后,用二氯甲烷提取。分析柱为C18反相柱,流动相为12.5 mmol/L四丁基硫酸氢铵乙腈溶液-磷酸盐缓冲液（10 mmol/LNa2HPO4,20 mmol/LKH2PO4,pH值3.50）（20/80）,柱温40℃,流速1 ml/min。[结果]在上述色谱条件下,克林霉素血浆提取液与空白血浆中其它杂质分离良好。克林霉素血浆浓度标准曲线线性范围为40-8 000 ng/ml,血浆中定量检测限为80 ng/ml（最低）,定性鉴定限为40 ng/ml,在80-8 000 ng/ml血浆浓度范围内具有良好的线性关系。总体回收率为（93.50±0.42）%,变异系数低于4.33%。在自动样器中存放24 h、30℃保存以及反复冻融均对克林霉素的稳定性无显著影响。[结论]该方法的选择性、灵敏度和色谱分辨率均很理想,可作为检测血浆中克林霉素的一种标准方法。
[Objective] The aim was to detect the clindamycin in rabbit plasma by HPLC/UV method.[Method] The serum samples were extracted by dichloromethane after the protein was deposited by acetonitrile.The analytical column was C18 reversed phase column,the mobile phase was acetonitrile solution containing 12.5 mmol/L tetra-n-butylam molonium hydrogen sulfate-phosphate buffer（contained 10 mmol/L Na2HPO4,20 mmol/L KH2PO4,pH=3.50）（20/80）,the column temperature was 40 ℃ and the flow rate was 1 ml/min.[Result] Under the above chromatographic conditions,the clindamycin plasma extract was better separated from other impurity in the blank plasma.The linear range of the concn.standard curve of the clindamycin plasma was 40-8 000 ng/ml,the limit of quantification in the plasma was 80 ng/ml（lowest） and the limit of qualitative detection was 40 ng/ml.There was a good linearity in the plasma concn.range of 80-8 000 ng/ml.The overall mean recovery value was（93.50±0.42）% and the coefficient of variation was lower than 4.33%.Storing in the automatic sampler for 24 h,preserving at 30℃,and repeated repeatedly freezing and thawing all had no significant influence on the stability of clindamycin.[Conclusion] The method all had ideal selectivity,sensitivity and chromatogram resolution and could be used as a standard method for detecting the clindamycin in the plasma.
出处
《安徽农业科学》
CAS
北大核心
2008年第27期11777-11779,共3页
Journal of Anhui Agricultural Sciences
