高效液相色谱法测定芒草^(60)Coγ辐照降解副产物

Using HPLC to determinate the main byproducts degraded by ^(60)Co γ irradiation on miscanthus

基于高效液相色谱法建立了同时定量分析芒草60Coγ辐照降解副产物(包括酚类、呋喃类和有机酸等9种)的方法。结果表明,采用C18色谱柱,柱温25℃,以乙腈–0.01 mol(NH4)2HPO4(用磷酸调节p H至2.7)为流动相,梯度洗脱,流速为0.8 m L/min,多波长紫外检测,可实现对目标化合物的有效分离和测定,相对标准偏差为1.5%~2.3%,最低检出限为0.10~0.89 mg/L。在该条件下对经1 200 k Gy 60Coγ辐照处理的芒草水提液进行检测,检测出水提液中目标化合物对羟基苯甲酸、香草酸、丁香酸、4–羟基苯甲醛、香草醛、对香豆酸、糠醛、甲酸、乙酸的质量浓度分别为17.78、12.43、3.26、15.40、10.18、16.42、2.52、102.29、86.24 mg/L。

An analytical method using high performance liquid chromatography（HPLC） for separation and quantitative determination 9 kinds of byproducts degraded by 60 Co γ irradiation on Miscanthus was developed. The separation was carried out on a C18 column with the following conditions： the mobile phase of acetonitrile and 0.01mol（NH4）2HPO4（phosphate adjust to p H=2.7）, 25 ℃ of column temperature, flow rate of 0.8 m L/min and multi-wavelength detection. The result showed that the byproducts of Miscanthus degraded from 60 Co γ irradiation were well separated and their contents were well determined with relative standard deviations from 1.5% to 2.3%, and detection limits varied from 0.10 to 0.89 mg/L. Water extracts of Miscanthus irradiated with 1 200 k Gy 60 Co γ were detected using the methods at above condition, it was found that the target chemicals in water extracts were included in p–hydroxybenzoic acid, vanillic acid, syringic acid, 4–hydroxybenza ldehyde, vanillin, p–coumaric acid, furfural, formic acid, and acetic acid, and their contents was 17.78 mg/L, 12.43 mg/L, 3.26 mg/L, 15.40 mg/L, 10.18 mg/L, 16.42 mg/L, 2.52 mg/L, 102.29 mg/L, and 86.24 mg/L, respectively. It was proved that the method was applicable to quantitative determination the main degradation byproducts of Miscanthus with 60 Co γ radiation pretreatment.