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

中文关键词:  胃蛋白酶  有机溶剂残留  气相色谱法

英文关键词:pepsin  residual organic solvents  gas chromatography

中文摘要:

      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, 0.25 μm), 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、80.0~400.0 μg/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。

英文摘要:

      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, 0.25 μm) 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?400.0 μg/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.