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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。
Objective To establish a method for the determination of formic acid in calcipotriol. Methods The gas chromatography was performed on a DB-624 capillary column (6% cyanopropylphenylpolysiloxane-94% dimethylpolysiloxane) with 0.53 mm × 30 μm and a liquid film thickness of 3.0 μm. Temperature 40 ℃, hold 5 min, at a speed of 10 ℃ .min-1 to 150 ℃; hold 10 min. Headspace injection, headspace bottle Balance temperature: 70 ℃, equilibration time: 30 min, injection volume of 1 ml. Nitrogen as a carrier gas, a flow rate of 3 ml.min-1; FID detector. Results Formic acid had a good linearity with a correlation coefficient greater than 0.999. The average recovery was 100.1%. The limit of detection was 1.19 mg.L-1. Conclusion The method is simple, sensitive, reproducible and accurate. It is suitable for the determination of formic acid residues in calcipotriol.