比较高效液相色谱法与液相色谱质谱联用方法测定大鼠肾脏中多黏菌素B的浓度

发布时间：2018-02-28 06:21

本文关键词： 高效液相色谱法大鼠肾组织多黏菌素B 液相色谱质谱联用方法　出处：《中国药学杂志》2015年10期 　论文类型：期刊论文

【摘要】：目的建立高效液相色谱紫外法测定大鼠肾脏组织中多黏菌素B的含量,并与液相色谱质谱联用方法测定的结果进行对比。方法色谱条件:色谱柱为Platisil ODS C18(4.6 mm×250 mm,5μm),流动相为乙腈-无水硫酸钠(7 g·L-1)-磷酸(6.8%,V/V)-水(22.25∶50∶5∶22.75),流速为1.0 m L·min-1,检测波长为205 nm,蛋白沉淀剂:磺基水杨酸。将多黏菌素B2.5 mg·kg-1连续2 d从尾静脉给予各组大鼠,然后分别给予4、8和16 mg·kg-1,连续给药3 d,检测大鼠肾脏中的多黏菌素B的浓度,并以LC-MS/MS进行结果验证。结果采用高效液相方法时,肾脏组织中多黏菌素B检测浓度线性范围为2~20μg·m L-1(r=0.997 8)。体外高、中、低3个浓度的绝对回收率在97%~102%之间;日内、日间精密度的RSD均小于5.0%;样品处理前后及反复冻融后稳定性的RSD均小于10%。高、中、低3个剂量组大鼠肾脏中药物含量分别为(86.16±3.28)、(47.40±0.51)、(21.48±1.63)μg·g-1。液相色谱质谱联用方法验证结果分别为(80.64±2.17)、(42.44±0.61)、(24.46±3.04)μg·g-1,两种方法检测结果的误差均在20%以内。结论本实验建立的高效液相色谱紫外法可用于检测大鼠肾脏中多黏菌素B的含量,其结果与液相色谱质谱联用方法测定的结果相似。
[Abstract]:Objective to establish a high performance liquid chromatography (HPLC) UV method for the determination of polymyxin B in rat kidney. The chromatographic conditions were as follows: the column was Platisil ODS C184.6 mm 脳 250mm ~ 5 渭 m ~ (-1), the mobile phase was acetonitrile-anhydrous sodium sulfate 7 g 路L ~ (-1) Phosphate 6.8g 路L ~ (-1) Phosphate 6.8g 路L ~ (-1) H _ 2O _ (22.25): 50: 522.755.The flow rate was 1.0 mL 路min ~ (-1), and the detection wavelength was 205nm. Protein precipitator: sulfosalicylic acid. The rats were given polymyxin B 2.5 mg 路kg-1 from the caudal vein for 2 days. The concentrations of polymyxin B in rat kidney were determined by LC-MS/MS for 3 days. The results were verified by LC-MS/MS. The linear range of polymyxin B in renal tissue was 20 渭 g 路ml ~ (-1) ~ 0.997 8 渭 g 路m ~ (-1) 路L ~ (-1) 路L ~ (-1). The absolute recovery of polymyxin B in vitro was in the range of 97 ~ 102%. The RSD of daytime precision is less than 5.0, the RSD of stability before and after sample treatment and after repeated freezing and thawing is less than 10. The contents of drugs in the kidney of the rats in the low dose groups were 47.40 卤0.51 卤1.63 渭 g 路g 路g-1.The results of HPLC / MS were 80.64 卤2.17 卤0.61 卤0.61 卤0.61 卤0.64 卤0.61 卤0.61 卤4.46 卤3.04 渭 g 路g -1, respectively. The errors of the two methods were within 20%. Conclusion High performance liquid chromatography was established in this experiment. The method can be used to determine the content of polymyxin B in rat kidney. The results are similar to those obtained by liquid chromatography-mass spectrometry.
【作者单位】：安徽医科大学空军临床学院;空军总医院药学部;
【分类号】：R927.2;O657.63

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