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目的建立毛细管气相色谱法测定羟乙基淀粉中2-氯乙醇的残留量。方法采用毛细管气相色谱法。色谱柱为DM-WAX弹性石英毛细管柱(30 m×0.25 mm,0.25μm);载气为氮气;检测器为ECD;进样口和检测器温度均为250℃;柱温为程序升温,初始温度90℃,保持12 min,以每分钟20℃升温至120℃,保持2 min。结果2-氯乙醇质量浓度在14.30~119.2μg.L-1内线性关系良好,r=0.997 6;回收率为98.4%(n=9);检测限为9.54×10-3ng;定量限为2.86×10-2ng。结论本法灵敏度高,简单,易行,结果准确可靠,可为羟乙基淀粉的质量控制提供依据。
Objective To establish a capillary gas chromatographic method for the determination of 2-chloroethanol in hydroxyethyl starch. Methods using capillary gas chromatography. The column was DM-WAX elastic quartz capillary column (30 m × 0.25 mm, 0.25 μm); the carrier gas was nitrogen; the detector was ECD; the inlet and detector temperatures were both 250 ℃; the column temperature was programmed temperature, initial The temperature was maintained at 90 ° C for 12 min and the temperature was raised to 120 ° C at 20 ° C per minute for 2 min. Results The linearity of 2-chloroethanol in the range of 14.30-119.2μg.L-1 was good, r = 0.997 6, the recovery was 98.4% (n = 9), the detection limit was 9.54 × 10-3ng, and the limit of quantification was 2.86 × 10-2ng. Conclusion The method is sensitive, simple and easy to operate with accurate and reliable results. It can provide the basis for the quality control of hydroxyethyl starch.