确定盐酸博宁霉素中成盐比例  

Determination of salt-forming proportion in boningmycin hydrochloride

作　　者：李娅萍[1] 陈汝贤[2] 杨亚莉[1] 胡昌勤[1] 

机构地区：[1]中国食品药品检定研究院,北京100050 [2]中国协和医科大学中国医学科学院医药生物技术研究所,北京100050

出　　处：《中国新药杂志》2013年第22期2616-2621,共6页Chinese Journal of New Drugs

基　　金：国家"重大新药创制"科技重大专项(2011ZX09303-001;2012ZX09301002-001);国家科技支撑计划(2012BAK25B02)

摘　　要：目的:采用新型混合模式离子交换柱建立新的HPLC-ELSD法确定一类新药盐酸博宁霉素中成盐比例。方法:采用HPLC-ELSD法,采用新型混合模式离子交换柱Acclaim Trinity P1(100 mm×3.0 mm,5μm),以30 mmol·L-1醋酸铵缓冲液(取醋酸铵4.59 g,加水1 900 mL使溶解,用冰醋酸调节pH至5.2,加入乙腈100 mL)-乙腈(50∶50)为流动相,流速为0.3 mL·min-1,柱温为25℃;蒸发光散射检测器的漂移管温度为90℃,氮气作为载气,流速为2.6 mL·min-1;分析18批盐酸博宁霉素中氯离子含量,折算成盐酸含量,并进行了方法学验证。结果:在19.0～308.7μg·mL-1范围内,氯离子浓度与峰面积呈对数相关关系(r=0.999 6),加样回收率分别为91.1%,99.4%,98.6%,RSD分别为2.3%,1.2%,1.3%(n=3),18批盐酸博宁霉素中氯离子含量折算成以盐酸计,平均含量为6.73%。结论:本研究新建的HPLC-ELSD方法专属性强、线性范围宽、耐用性好,通用性很好,能适用于测定盐酸博宁霉素中氯离子含量,进而折算成盐酸含量,在此生产条件下,博宁霉素与盐酸成盐比例为1∶3。Objective： To establish a new HPLC-ELSD method to determine the salt-forming proportion in the new drug boningmycin hydrochloride using a new type of mixed-mode ion exchange column. Methods： The content of chloride in boningmycin hydrochloride was analyzed by a new HPLC-ELSD method which was equipped with a new type of mixed-mode ion exchange column named as Acclaim Trinity P1 （100 mm x 3.0 mm, 5 um） and an ELSD detector. A mixture of 30 mmol- L- 1 ammonium acetate buffer （4.59 g of ammonium acetate dissolved in I 900 mL of water, pH value adjusted to 5. 2 with glacial acetic acid, and 100 mL of acetonitrile）-acetonitrile （50： 50） was used as mobile phase. The flow rate was 0.3 mL rain- The column temperature was set at 25 ℃. The temperature of drift tube in an evaporating light scattering detector was 90 ℃. Nitrogen gas was used as carrier gas and the flow rate was 2.6 mL per minute. The chloride contents in 18 lots of boningmycins hydrochloride were analyzed and converted to the content of hydrochloride. The method was validated adequately. Results： The con-centration of chloride was logarithmically related with the peak area from 19.0 to 308.7 Dxg mL-I （ r = 0. 999 6）. The spiked recoveries were 91.1%, 99.4% and 98.6%, and RSDs were 2. 3% , 1.2% andl.3% （n=3）. The average content of hydrochloride in 18 lots of boningmycin hydrochloride was 6.73%. Conclusion： The new HPLC- ELSD method is specific, linear, accurate, precise and robust for determination of the chloride content in boningmy- cin hydrochloride. The salt-forming proportion in boningmycin hydrochloride is 1：3 in the prescribed process.

关 键 词：盐酸博宁霉素 成盐比例 氯离子含量 HPLC—ELSD 

分 类 号：R927.2[医药卫生—药学] R979.14