胶束电动毛细管电泳分析紫杉醇的主成分含量

Main component analysis of paclitaxel by micellar electrokinetic capillary chromatography

目的:建立胶束电动毛细管电泳(MECC)分离测定紫杉醇的新方法。方法:以40.2 cm×50μm(到检测窗口的有效长度30 cm)的熔融石英毛细管柱为分离柱、V(10 mmol/L三羟甲基氨基甲烷+140 mmol/L十二烷基硫酸钠+70 mmol/L硼酸+40 mmol/L羟丙基-β-环糊精):V(甲醇+异丙醇)=1:1(其中V(甲醇):V(异丙醇)=1:1)为分离缓冲液,于203 nm处检测。结果:方法的精密度为0.08%(n=7),检出限为1.5 mg/L(S/N=3),定量限为4.5 mg/L(S/N=10),1200 mg/L紫杉醇的迁移时间的相对标准偏差(RSD)为0.18%,峰面积的RSD为2.5%。用校正峰面积归一化法测定了纯化后的紫杉醇的主成分含量,并与高效液相色谱(HPLC)的测定结果进行了比较。

Objective：To develop a new method for the main component analysis of paclitaxel by micellar electrokinetic capillary chromatography（MECC）.Methods：The separation was carried out with an uncoated fused-silica capillary with 50 μm i.d.and total length of 40.2 cm（the effective length to the detector was 30 cm）.The optimized separation buffer was as follows： V（10 mmol/L Tris（hydroxymethyl） aminomethane＋140 mmol/L sodium dodecyl sulfate＋70 mmol/L boric acid＋40 mmol/L hydroxypropyl-cyclodextrin）： V（methanol＋isopropa nol）=1：1.The proportion of methanol and isopropanol was optimized to be 1： 1.The paclitaxel was detected at 203 nm.Results：The precision of the method was 0.08%（n=7）.The limit of detection（LOD） was 1.5 mg/L（S/N=3）.The limit of quantitation（LOQ） was 4.5 mg/L（S/N=10）.The relative standard deviation（RSD） values for migration time and peak area of 1200 mg/L paclitaxel were 0.18% and 2.5%（n=7）,respectively.The content of the main component of the purified paclitaxel was analyzed by correctedly normalized area,and the results were compared with those of high performance liquid chromatographic method（HPLC）.