毛细管气相色谱法检测生长抑素中有机溶剂残留量

目的：建立生长抑素中4种有机溶剂残留量的分离测定方法。方法：采用直接进样毛细管气相色谱法，程序升温，色谱柱为DB-624毛细管柱，载气为氮气，FID检测器，双蒸水为溶解介质，检测了生长抑素原料药中乙腈、哌啶、醋酸、Ⅳ，Ⅳ-二甲基甲酰胺的残留量。结果：4种有机溶剂完全分离，在所考察的浓度范围内具有良好线性，r为0．9997—1．000，乙腈、哌啶、醋酸、Ⅳ，Ⅳ-二甲基甲酰胺的检测限分别为0．3，2．2，1．3，0．4ng，精密度RSD均小于5％，平均回收率为103．3％-105．6％。结论：本试验建立的方法简便灵敏，结果准确可靠，适用于生长抑素中有机溶剂残留量的检测。

Determination of Residual Solvents in Somatostatin by Capillary Gas Chromatography

Objective:To establish a method for determination of four residual solvents in somatostatin.Method: The residual solvents which are acetonitrile,piperidine,acetic acid,N,N-dimethylformamide (DMF)were quantita- tively determined by capillary GC on DB-624 column,water as solvent media,with FID detector,nitrogen as the carrier gas.Results:Four residual solvents were completely separated.There was a good linearity (r:0.9997- 1.000).The detection limit of acetonitrile,piperidine,acetic acid and DMF were 0.3,2.2,1.3,0.4 ng;the RSD of precision was less than 5%;the average recovery rate of the preparation was in the range of 103.3%-105.6%. Conclusion:The method is simple,sensitive,accurate and can be used for the quality control of somatostatin.