毛细管气相色谱法测定卡泊三醇中甲酸残留量

目的建立卡泊三醇中甲酸的含量测定方法。方法使用气相色谱仪,采用DB-624毛细管色谱柱(6%氰丙基苯聚硅氧烷-94%二甲基聚硅氧烷),0.53 mm×30 m,液膜厚度为3.0μm;柱温40℃,保持5 min,以10℃.min-1的速度升温至150℃;保持10 min。顶空进样,顶空瓶平衡温度:70℃,平衡时间:30 min,进样量为1 ml。以氮气为载气,流速为3 ml.min-1;FID检测器。结果甲酸线性关系良好,相关系数大于0.999;平均回收率为100.1%;检出限为1.19 mg.L-1。结论该方法简便,灵敏度高,重复性好,结果准确,适合于卡泊三醇中甲酸残留量的测定。

Determination of formic acid in calcipotriol by GC

Objective To establish a GC method for determination of formic acid of calcipotriol.Methods DM-624 capillary column（0.53 mm×30 m×3.0 μm,coated with 6% cyanopropylplysiloxane phenyl and 94% dime-thylpolysiloxane） was adopted and the carrier gas was nitrogen with 3 ml·min-1 of flow rate.The initial column temperature was kept at 40 ℃ for 5 min,then raised to 150 ℃ and kept for 10 min at the rate of 10 ℃·min-1.Head-space injection,equilibration temperature was 70℃,equilibration time is 20 minutes and injection volume was 1.0 ml.FID detection was adopted.Results The correlation coefficient of formic acid was higher than 0.999.The recovery was 100.1% and limit of detection was 1.19 mg·L-1.Conclusion This method is sensitive,accurate,repeatable and easy to operate for determination of formic of calcipotriol.