毛细管气相色谱法测定异黄酮衍生物2702中有机溶剂残留量

Determination of Residual Organic Solvents from Isoflavone Derivate 2702 by Cappillary Gas Chromatography

建立异黄酮衍生物2702中乙醇,乙酸乙酯残留量的测定方法。采用毛细管气相色谱法,色谱柱为DB-Wax(30m×0.45mm×0.85μm)石英毛细管柱;检测器为FID,载气为氮气;柱温为程序升温:起始温度为40℃,保持5min,然后以40℃/min的速率升至205℃,保持8min;气化室温度为225℃。在该色谱条件下,采用甲苯为内标。测得乙醇、乙酸乙酯二种溶剂分别在1.25～87.50μg/mL(r=0.9998);1.80～89.90μg/mL(r=0.9999)范围内线性关系良好,平均回收率分别为102.0%(RSD=2.8%),98.4%(RSD=2.3%);检测限分别为0.13ng,0.17ng。因此,该毛细管气相色谱法简单、结果准确,适用于本品有机溶剂残留量的测定。

To establish a method for determination of residual organic solvents in isoflavone derivate2702, a capillary GC method was developed with DB-Wax （30 m × 0.45 mm × 0.85 μm） quartzose capillary column with FID detector and nitrogen as the carrier gas; the column temperature was raised by program, the initial temperature was 40℃ for 5 min, then the temperature was raised to 205℃ at the rate of 40℃/min, maintain for 8 min;the injector temperature was 225℃; The content was calculated by internal standard method. The analytical balidation for each residual organic solvents was performed, The calibration curves linear of ethanol and ethylacetate was linear in the concentration ranger 1.25 - 87.50 μg/mL and 1.80 - 89.90 μg/mL and the correlation coefficient was 0.999 8 and 0.999 9. The average recoveries were 102.0% and 98.4% respectively with RSD of 2.8% and 2.3 % ; the limit of detection were 0.13 ng and 0. 17 ng respectively. This GC method was proved to be accurate, sensitive, reliable and suitable for the residual solvents detection of isoflavone derivate. The results was accord with the request of pharmacopeia.