摘要
目的建立RP-HPLC测定血浆中溴吡斯的明浓度的方法。方法采用Sep-Pak柱固相萃取法提取溴吡斯的明;Waters2690系列高效液相色谱仪测定。色谱柱Nucleosil 100-5 CN柱(4.6 mm×250 mm,5μm);柱温:室温;检测波长:269 nm;流动相为乙腈-水(0.1%三乙胺水溶液加1 mol.L-1HAc调节pH3.2)梯度洗脱;外标法定量。结果溴吡斯的明血药浓度的线性范围为2.0～50.0μg.L-1;最低检测浓度2.0μg.L-1;方法回收率为96.89%～111.51%;日内及日间精密度分别为2.79%～7.00%和2.33%～5.51%。结论本法灵敏、准确,可用于溴吡斯的明人体药动学研究。
OBJECTIVE To establish a RP-HPLC method for the determination of pyridostigmine bromide in human plasma, METHODS The drug was extracted from plasma with Sep-pak column by SPE method. The compounds were separated on a Nucleosil 100 -5 CN column（4. 6 mm×250 mm,5μm） by Waters 2690 HPLC. The mobile phase was a mixture of acetonitrile-water （0.1% triethylamine solution adjusted to pH 3, 2 with 1 mol·L^-1 acetic acid ） using a gradient. The detection wavelength was 269 nm. The external standard method was used for quantitative analysis. RESULTS A good linearity was obtained over the range of 2. 0 - 50.0μg·L^-1. The limit of detection was 2, 0 μg·L^-1 The recoveries of method were from 96. 89% to 111.51%, The precisions of intra-day and inter-day were 2, 79% -7. 00% and 2, 33% -5, 51% ,respectively. CONCLUSION The method is sensitive, accurate and reliable, and can be used in clinical research of pyridostigmine bromide.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2007年第12期924-926,共3页
Chinese Pharmaceutical Journal
