中国临床药学杂志

目的建立用于检测糜蛋白酶原料药中磷酸三丁酯残留量的毛细管气相色谱法。方法供试品采用正己烷提取,内标法测定。TM-FFAP毛细管柱,载气为高纯氮气,正己烷为溶解介质,柱温为恒温160℃,进样口温度为200℃,检测器温度为230℃,进样量1.0μL,分流进样,分流比1∶5,FID检测器。结果被测物磷酸三丁酯在所考察的浓度范围内呈现良好线性关系,r=0.996 6,平均回收率为96.28%~103.54%,精密度的RSD<5%,完全符合残留溶剂测定的技术要求。结论本试验建立的方法简单、准确、精密度高,可用于糜蛋白酶中磷酸三丁酯残留量的测定。

AIM To establish a method for determination of tributyl phosphate residual solvent in chymotrypsin by capillary gas chromatography.METHODS The sample was extraced with n-hexane,and internal standard method was used for the determination.The residual solvent of tributyl phosphate was quantitatively determined by capillary gas chromatography on TM-FFAP column with n-hexane as solvent media and high purity nitrogen as the carrier gas.The oven's temperature was constant temperature on 160 ℃,inlet's was 200 Tl,and detector's was 230 ℃.Sample size was1.0 μL,split sampling and split ratio was 1:5,with FID detector.RESULTS There was a good linearity(r =0.996 6),and the average recovery rate of the preparation was in the range of 96.28%- 103.54%.The RSD of precision was less than 5%.They were in complete accord with specifications of residual solvent determination.CONCLUSION The method is simple,rapid and sensitive,and can be used in the determination of tributyl phosphate residual solvent for the quality control of chymotrypsin.