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建立了区带毛细管电泳法分离测定原料药及其缓释胶囊中坦索罗辛和有关中间体的方法。采用未涂层石英毛细管(75μm i.d.×60 cm,有效长度50cm),以20 mmol/L硼砂(pH7.30)为运行缓冲液,检测波长230nm,阳极端压力自动进样10s(3.4kPa),分离电压15kV,温度25℃。坦索罗辛及其中间体在7 min中内得以基线分离,坦索罗辛在10.28~123.4μg/mL(r=0.9995),(R)-5-(2-氨基丙基)-2-甲氧苯基磺酰胺在14.99~179.9μg/mL(r=0.9993),2-(2-乙氧苯氧基)溴乙烷在8.496~101.9μg/mL(r=0.9987)范围内线性关系良好,平均回收率分别为100.9%,100.1%和99.2%,平均RSD≤2.9%。方法为坦索罗辛缓释胶囊的测定和监测其合成生产过程提供了分析手段。
A method for the separation and determination of tamsulosin and its related intermediates by bulk capillary electrophoresis in pharmaceutical raw materials and their sustained-release capsules was established. Uncoated quartz capillary tube (75 μm id × 60 cm, effective length 50 cm) was used as the running buffer with 20 mmol / L borax (pH 7.30). The detection wavelength was 230 nm and the pressure at the anode was automatically injected for 10 s (3.4 kPa) Separation voltage 15kV, temperature 25 ℃. Tamsulosin and its intermediates were baseline separated within 7 min with tamsulosin at 10.28-123.4 μg / mL (r = 0.9995), (R) -5- (2-aminopropyl) -2- There was a good linear relationship between methoxyphenylsulfonamide and choline in the range of 14.99-179.9μg / mL (r = 0.9993) and 2- (2-ethoxyphenoxy) ethyl bromide in the range of 8.496-101.9μg / mL The average recoveries were 100.9%, 100.1% and 99.2% respectively, with an average RSD ≤ 2.9%. The method provided an analytical tool for the determination of tamsulosin sustained-release capsules and for the monitoring of its synthetic production process.