气相色谱法测定合成产物中诺蒎酸的含量

GC Determination of Nopinic Acid in the Products of Its Synthesis

摘要: 采用气相色谱法跟踪测定了β-蒎烯氧化反应中主产物诺蒎酸的含量;试验结果表明,在SE-30/Chromosorb W/AW(0.25~0.175 mm)的色谱柱上,诺蒎酸与副产物之间具有较好的分离效果,并且在峰形对称性和出峰时间上,SE-30柱也具有优势;该方法的线性范围在15.0~60.0 g·L-1之间,检出限(S/N=3)为3.5 g·L-1;对同一试样的5次平行测定的相对标准偏差为1.8%;该方法的标准加入回收率达90%~98%.

Abstract: Nopinic acid was synthesized from β-pinene by oxidation with KMnO4 in alkaline solution,and amount of nopinic acid in the reaction products was determined by gas chromatograph with the SE-30/chromosorb W/AW separation column (0.25-0.175 mm).By use of the proposed column,nopinic acid was nicely separated from the by-products,and well-difined symmetrically shaped peak of nopinic acid was obtained.Linear relationship between peak area and mass concentration of nopinic acid was obtained in the range from 15.0 to 60.0 g·L-1,with detection limit (S/N=3) of 3.5 g·L-1.Recovery and precision of the method were tested,giving value of RSD (n=5) of 1.8% and values of recovery in the range of 90%-98%.