离子色谱法测定盐酸平阳霉素中的氯离子

Determination of chloridion in bleomycin A_5 hydrochloride by ion chromatography

目的建立离子色谱法测定盐酸平阳霉素中的氯离子含量，推测其成盐比例。方法采用Dionex IonPac AS11-HC（250mm×4mm，5μm）为色谱柱，以20mmol／L氢氧化钠溶液为淋洗液，流速为1．0mL／min，柱温为30℃，检测池温度为35℃，抑制性电导检测器的抑制电流为100mA；测定3批盐酸平阳霉素中氯离子的含量，换算出盐酸含量，并进行了方法学验证。结果在2～30μg／mL浓度范围内，氯离子溶液的峰面积与其浓度呈良好的线性关系（r=1.0000），加样回收率分别为98．6％、99．5％和99．5％；RSD分别为0．82％、0．21％~10．45％（n=3），3批盐酸平阳霉素中氯离子的含量折算成以盐酸计，平均含量为6．83％。结论本研究建立的离子色谱法操作简单，线性范围、重复性、回收率好，能适用于测定盐酸平阳霉素中氯离子含量，进而得到平阳霉素与盐酸成盐比例为1：3。

Objective To establish a method to speculate the salt-forming proportion in bleomycin A5 by ion chromatography. Method A Dionex IonPac AS11-HC （250mm×4mm,5μm） column was used. The elutriant was 20mmol/L sodium hydroxide solution. The flow rate was 1.0mL/min. The column temperature was set at 30℃. Inhibitory electrical detector was used with detecting pool temperature of 35℃. The chloride contents in 3 lots of bleomycin A5 hydrochloride were analyzed and converted to the content of hydrochloride. The method was validated adequately. Results The calibration curve was linear in the range of 2-30μg/mL for concentration of chloride（r=1.0000）. The spiked recoveries were 98.6%, 99.5% and 99.5%, and the RSDs were 0.820,0.21% and 0.45%（n=3）. The average content of hydrochloride in 3 lots of samples was 6.83%. Conclusion The method is simple, linear, accurate, precise and suitable for the determination of chloride content in bleomycin A5 hydrochloride. The salt-forming proportion in bleomycin A5 hydrochloride is 1：3.