摘要
目的:建立测定聚明胶肽注射液中残留交联剂1,4-环己烷二异氰酸酯水解产物1,4-环己烷二胺含量的方法。方法:采用HPLC-FLD法,衍生化试剂:丹磺酰氯,色谱柱:YMC C18柱(250 mm×4.6 mm,5μm),流动相:甲醇-水(80:20),检测器:荧光检测器(激发波长:340 nm,发射波长:515 nm),流速:1.0 ml·min^(-1),柱温:35℃,进样量:20μl。结果:制剂中其他成分无干扰,反式1,4-环己烷二胺在0.282～5.640μg·ml^(-1)(r=0.999 9)范围内的质量浓度与其双酰化衍生物峰面积的线性关系良好,顺式1,4-环己烷二胺在0.298～5.960μg·ml^(-1)(r=1.000 0)范围内的质量浓度与其双酰化衍生物峰面积的线性关系良好;反式和顺式1,4-环己烷二胺的平均回收率分别为100.32%(RSD=1.52%,n=6)、99.62%(RSD=1.48%,n=6),测得各批聚明胶肽注射液中的1,4-环己烷二胺总含量均低于5μg·ml^(-1)。结论:该分析方法灵敏度高、准确、专属性强,重复性好,可用于测定聚明胶肽注射液中环己烷二胺残留量的测定。
Objective： To develop an HPLC-FLD method for the determination of 1,4-diaminocyclohexane,a hydrolyte of the residual cross-linking agent 1,4-cyclohexane diisocyanate（ CHDI） in polygeline injection. Methods： The detection was performed by HPLC-FLD on a YMC C_（18） chromatographic column（ 250 mm × 4. 6 mm,5 μm）. The derivatization reagent was dansyl chloride,and the mobile phase was methanol-water（ 80： 20）. A fluorescence detector was used,the excitation wavelength was 340 nm,and the emission wavelength was 515 nm. The flow rate was 1. 0 ml· min-1,the column temperature was 35℃,and the injection volume was20 μl. Results： There was no interference from the other substances in the preparation. The linear range of trans-1,4-diaminocyclohexane concentration was 0. 282-5. 640 μg · ml^（-1）（ r = 0. 999 9）. The linear range of cis-1,4-diaminocyclohexane concentration was0. 298-5. 960 μg · ml-1（ r = 1. 000 0）. The mean recovery of trans-1,4-diaminocyclohexane and cis-1,4-diaminocyclohexane was100. 32%（ RSD = 1. 52%,n = 6） and 99. 62%（ RSD = 1. 48%,n = 6）,respectively. The content of 1,4-diaminocyclohexane was less than 5 μg·ml^（-1） in all the tested samples. Conclusion： The method is sensitive,accurate,specific and reproducible,and suitable for the determination of 1,4-diaminocyclohexane and the control of the residual cross-linking agent in polygeline injection.
作者
毛芬兰
干伟
干国平
刘澍秾
管子琪
Mao Fenlan;Gan Wei;Gan Guoping;Liu Shunong;Guan Ziqi(College of Pharmacy, Hubei University of Traditional Chinese Medicine, Wuhan 430065, China;Hubei Shu Connaught Pharmaceutical Co. Ltd.)
出处
《中国药师》
CAS
2018年第4期727-730,共4页
China Pharmacist
