气相色谱法测定伊潘立酮中1-溴-3-氯丙烷的残留

目的建立1-溴-3-氯丙烷在伊潘立酮中的Gc检测方法。方法样品采用DMF萃取。色谱系统采用DM-624（30m×0．53μm×3．0μm）气相色谱柱，柱温为程序升温．氢火焰离子化检测器（FID），分流比为3：1。结果1-溴-3-氯丙烷在37．5～87．5ng·mL-1内进样，按外标法以峰面积计呈良好的线性关系，平均回收率为99．4％。RSD为0．31％（n=9），精密度RSD为0．89％（n=6），最低检测浓度为12．5ng·mL-1，可检测出样品中含有12．5ppm的1-溴3-氯丙烷。结论该方法简便、准确，重复性好，适用于伊潘立酮的质量控制和检测。

Determination of Residues of 1-bromine-3-chloropropane in Iloperidone by Gas Chromafography

OBJECTIVE To establish a gas chromatography （GC） method for determination of residues of !-bro- mine-3-chloropropane in iloperidone. METHODS The samples were extracted by DMF. The content of 1-bromine- 3-chloropropane was detected by FID after the separation in a DM-624 column（30m ×0.53mm × 3.0μm）. Column temperature was increased by programmed control and split flow of 3： 1. RESULTS The calibration cure was linear over the range of 37.5 - 87.5ng ·mL -1, the average recovery of 99.4%, RSD was 0. 31% （ n = 9 ） ; RSD of precision was 0. 89% （n = 6 ）, the lowest detection limit was 12. 5ppm 1-bromine-3-chloropropane, the minimum detection con- centration was 12.5ng · mL-1. CONCLUSION The method is sample,accurate,reproducible and applicable to the iloperidone of quality control and detection.