气相色谱法测定胃蛋白酶中7种有机溶剂残留

Determination of 7 kinds of residual organic solvents in pepsin by gas chromatography

目的建立测定胃蛋白酶原料中7种有机溶剂残留的气相色谱法(gas chromatography,GC)。方法样品以纯化水为溶剂,80℃顶空加热20 min,采用DM-Wax毛细管色谱柱(30 m×0.32 mm,0.25μm),程序升温对有机溶剂进行分离,氢火焰离子化检测器(flame ionization detector,FID)检测,外标法定量。结果乙醛、正丙醛、丙酮、甲醇、正丙醇、异丙叉丙酮、二丙酮醇分别在质量浓度为1.8~9.0、1.65~8.25、60.0~300.0、33.0~165.0、10.0~50.0、2.0~10.0、80.0~400.0μg/mL范围内线性关系良好,相关系数(r)均大于0.9995。方法平均回收率分别为97.6%、94.2%、98.7%、95.9%、95.6%、95.5%、94.4%,相对标准偏差为1.20%、0.91%、1.30%、1.30%、0.62%、0.93%、1.70%。结论该方法前处理简单,具有较好的准确性、灵敏度和精密度,增加了监测溶剂的种类,适用于胃蛋白酶原料中溶剂残留量的检测。

Objective To establish a method for the determination of 7 kinds of residual organic solvents in pepsin raw materials by gas chromatography(GC).Methods Purified water was used as the solvent and heated in headspace at 80℃for 20 min,DM-Wax capillary column(30 m×0.32 mm,0.25μm)was used,the organic solvent was separated by temperature-programmed,detected by flame ionization detector(FID),and quantified by external standard method.Results Acetaldehyde,propionaldehyde,acetone,methanol,n-propanol,isopropylidene acetone and diacetone alcohol showed good linear relationships in the mass concentrations ranges of 1.8‒9.0,1.65‒8.25,60.0‒300.0,33.0‒165.0,10.0‒50.0,2.0‒10.0,80.0‒400.0μg/mL,respectively,and the correlation coefficients(r)were all greater than 0.9995.The average recoveries of the method were 97.6%,94.2%,98.7%,95.9%,95.6%,95.5%and 94.4%,respectively,the relative standard deviations were 1.20%,0.91%,1.30%,1.30%,0.62%,0.93%and 1.70%,respectively.Conclusion This method has advantages of simple pretreatment,good accuracy,sensitivity and precision,and increases the types of monitoring solvents,it can be used for the detection of solvent residues in pepsin raw materials.