高效毛细管电泳法测定盐酸芦氟沙星制剂的含量

HPCE Determination of Rufloxacin Hydrochloride Preparations

目的:建立一种高效毛细管电泳(HPCE)分析方法,用于盐酸芦氟沙星制剂的含量测定,并与高效液相色谱法(HPLC)进行比较。方法:以75μm×365μm(总长62 cm,有效长度53.5 cm)熔融石英毛细管为分离通道,20 mmol·L^(-1)硼酸盐-25mmol·L^(-1)磷酸盐缓冲液(pH 8.7)为电泳缓冲液,运行电压18 kV,柱温28℃,紫外检测波长295 nm;分别采用外标法和内标法定量,HPLC 法采用外标法定量。结果:外标法:盐酸芦氟沙星在1.4×10^(-6)～5.7×10^(-5)mol·L^(-1)浓度范围内线性关系良好(r=0.9997),检测限5×10^(-7)mol·L^(-1),定量限1.4×10^(-6)mol·L^(-1),日内和日间峰面积的 RSD 分别为1.02%～1.73%和1.90%～3.84%,加样回收率为99.6%(98.5%～100.5%,胶囊)和99.4%(98.6%～100.1%,片剂);内标法:盐酸芦氟沙星在1.6×10^(-6)～1×10^(-4)mol·L^(-1)浓度范围内线性关系良好(r=0.9997),检测限5.1×10^(-7)mol·L^(-1),定量限1.6×10^(-6)mol·L^(-1),日内和日间药物峰面积与内标峰面积之比的 RSD 分别为0.84%～1.33%和1.83%～2.40%,加样回收率为100.3%(99.2%～102.0%,胶囊)和99.5%(99.4%～99.6%,片剂)。结论:所建立的 HPCE 法简便、快速、经济,外标法和内标法测定结果准确度高、重复性好,且与 HPLC 法测定结果一致,均可作为盐酸芦氟沙星胶囊和片剂的质量控制方法。

Objective：To establish an analytical method of high performance capillary electrophoresis （HPCE） to determine the content of rufloxacin hydrochloride preparations and compare HPCE method with the method of high performance liquid chromatography （HPLC）. Methods：The determination was performed on a fused silica capillary （75 μm × 365 μm ,62 cm in total length and 53.5 cm to the detector）. Optimized analytical conditions are as follows ： running buffer system of 20 mmol · L ^- 1 borate - 25 mmol · L^ - 1 phosphate buffer with pH 8.7,18 kV applied voltage,temperature 28 ℃ and UV detection at 295 nm. The external standard method （ ESM ） and the internal standard method （ISM） were used as the quantitative methods of HPCE. ESM was used as the quantitative method of HPLC. Results：The linearity range is 1.4 × 10^-6 -5.7 × 10 ^-5mol · L^-1 （r =0. 9997） for ESM and 1.6 × 10^ -6- 1 × 10^ -4mol · L^-1 （r = 0. 9997 ） for ISM. The detection limit and the quantification limit of rufloxacin hydrochloride is 5 × 10^-7mol · L^-1 and 1.4 × 10^-6mol · L^-1 respectively for ESM,and 5.1 × 10^-7mol · L^-1 and 1.6 × 10^-6mol · L^-1 respectively for ISM. The quantitative precision of ESM is 1.02% - 1.73% for intra - day and 1.90% - 3.84% for inter- day,and that of ISM 0.84% -1.33% for intra -day and 1.83% -2.40% for inter -day. The recovery of ESM is 99.6% （98.5% - 100.5% ） for capsules and 99.4% （98.6% - 100. 1% ） for tablets. The recovery of ISM is 100. 3% （99.2% - 102.0% ） for capsules and 99.5% （99.4% -99.6% ） for tablets.. Conclusions ： HPCE method is much more simple, rapid and economic than HPLC method. Moreover, the results determined by HPCE method （ESM and ISM） are exact,reproducible and consistent with that determined by HPLC method. So HPCE method can be used to control the quality of rufloxacin hydrochloride capsules and tablets.