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Title:: Determination of epichlorohydrin residues in hemostatic granules of carboxymethyl starch

Author(s):: ZHU Xiaomin; ZHU Xiaojie; MENG Jianwen; LI Hongmei; ZHANG Suwen; HOU Xiuju; Shandong Academy of Pharmaceutical Science，Shandong Provincial Key Laboratory of Biomedical Polymer，Jinan 250101，China

Keywords:: Carboxymethyl starch; Hemostatic granules; Headspace gas chromatography; Residual epichlorohydrin; Detection

摘要:: 本研究建立了顶空气相色谱法测定羧甲基交联淀粉止血颗粒中环氧氯丙烷残留量的方法。使用Agilent DB-624（30 m×530 μm×3.0 μm）毛细管色谱柱，柱温为程序升温（50℃，保持2 min；50℃/min升温至180℃，保持5 min），进样口温度为200℃，检测器温度为250℃，载气为N2，流速为3 mL/min，分流比为3∶〖KG-*2/3〗1。精密度相对标准偏差为1.22%；环氧氯丙烷的浓度为0.84~6.72 μg/mL，其峰面积与浓度线性关系良好，相关系数为0.9997；检测限为0.336 μg/mL，定量限为0.84 μg/mL；平均回收率为101.7%（n=9）。该方法重现性好，灵敏度高，简单准确。

Abstract:: The residual epichlorohydrin in hemostatic granules of carboxymethyl starch was determined by headspace GC. Agilent DB-624 capillary column (30 m×530 μm×3.0 μm) was used,the initial column temperature was 50℃,Keep it for 2 minutes. Then the temperature was rised to 180℃ by 50℃/min,kept it for 5 min. The inlet temperature was 200℃. The detector temperature was 250℃. The carrier gas was N2 with a flow rate of 3 mL/min, and the shunt ratio was 3∶〖KG-*2/3〗1. The peak area and concentration of epichlorohydrin showed good linearity in the range of 0.840-6.72 μg/mL, and the correlation coefficient was 0.9997. The detection limit was 0.336 μg/mL and the quantitative limit was 0.840 μg/mL. The average recovery was 101.7% (n=9). The method is simple and accurate.