气相色谱法测定苯甲酸中有关物质的含量

目的： 建立测定苯甲酸中有关物质甲苯、苯甲醛、苯甲醇、联苯、2-甲基联苯、3-甲基联苯、4-甲基联苯、苯甲酸苄酯含量的方法。方法： 采用气相色谱法，色谱柱为Aglient DB-FFAP毛细管柱（30 m×0.32 mm，0.25 μm），柱温为程序升温（起始温度100℃，保持1 min，再以5℃·min^-1升温至230℃，保持5 min），氢火焰离子化检测器（FID），进样口温度270℃，检测器温度300℃，载气（N₂）流速为1.0 mL·min^-1，分流比10：1，进样量1 μL。结果： 甲苯、苯甲醛、苯甲醇、联苯、2-甲基联苯、3-甲基联苯、4-甲基联苯、苯甲酸苄酯分别质量浓度在0.258~77.413、0.223~66.953、0.237~71.137、0.182~54.512、0.263~78.863、0.288~86.342、0.164~49.062、0.232~69.500 μg·mL^-1范围内与各自峰面积积分值呈良好的线性关系，相关系数r均大于0.999，平均回收率均在95.5%~100.4%之间。样品中有关物质测定结果显示部分样品检出苯甲醛、苯甲醇、联苯、2-甲基联苯、3-甲基联苯、4-甲基联苯、苯甲酸苄酯等，检出值均较小，范围为0.001%~0.026%。结论： 该方法可用于苯甲酸有关物质的控制。

Objective: To establish a method for the determination of related substances(methylbenzene,phenylaldehyde,benzyl alcohol,biphenyl,2-methyl biphenyl,3-methyl biphenyl,4-methyl biphenyl and benzyl benzoate)in benzoic acid. Methods: GC method was adopted. The determination was performed on capillary column of Aglient DB-FFAP(30 m×0.32 mm,0.25 μm);the detector was FID;inlet temperature was 270℃;the detector temperature was 300℃;the column temperature was programmed to start at 100℃,maintained for 1 min,and then rose to 230℃ at a rate of 5℃·min^-1,maintained for 5 min;nitrogen(1.0 mL·min^-1)was used as the carrying gas;the split ratio was 10:1;the injection volume was 1 μL. Results: Methylbenzene,phenylaldehyde,benzyl alcohol,biphenyl,2-methyl biphenyl,3-methyl biphenyl,4-methyl biphenyl and benzyl benzoate showed good linear relationships within the ranges of 0.258-77.413 μg·mL^-1,0.223-66.953 μg·mL^-1,0.237-71.137 μg·mL^-1,0.182-54.512 μg·mL^-1,0.263-78.863 μg·mL^-1,0.288-86.342 μg·mL^-1,0.164-49.062 μg·mL^-1 and 0.232-69.500 μg·mL^-1,respectively with the correlation coefficients of above 0.999. And the average recoveries were 95.5%-100.4%. The determination results of the related substances showed that the amounts of phenylaldehyde,benzyl alcohol,biphenyl,2-methyl biphenyl,3-methyl biphenyl,4-methyl biphenyl and benzyl benzoate in some samples were small with the range of 0.001%-0.026%. Conclusion: This method can be used for the quality control of related substances in benzoic acid.

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