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高效液相色谱和离子色谱测定水中短链脂肪酸的方法比较 |
Comparison of ion chromatography and high-performance liquid chromatography for short-chain fatty acids determination |
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DOI: |
中文关键词: 离子色谱法 高效液相色谱法 短链脂肪酸 方法比较 |
英文关键词:ion chromatography high-performance liquid chromatography short-chain fatty acid method comparison |
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中文摘要: |
从分离谱图、分析时间、线性范围、检出限、精密度和加标回收率角度,对离子色谱和高效液相色谱(HPLC)测定水中的短链脂肪酸的方法进行比较。HPLC使用SunFireTM C18色谱柱,流动相为磷酸二氢钾溶液和甲醇,梯度洗脱,流速1.0 mL/min。离子色谱法使用DionexTM ATC-3色谱柱,流动相为不同浓度氢氧化钠溶液梯度洗脱,流速1.5 mL/min。结果表明:HPLC的分析时间、线性范围、检出限、保留时间精密度、峰面积精密度和加标回收率分别为14.5 min、0~1 200 mg/L、1557~23.23 mg/L、0.079%~0.597%、1.12%~3.50%和96.1%~112.0%,离子色谱法的相应指标分别为13.0 min、0~20 mg/L、0.03~0.10 mg/L、0.000%~0.053%、1.18%~2.69%和982%~122.0%。HPLC线性检测范围宽,但检出限相对高。离子色谱法检出限低,但线性检测范围窄,过高的进样质量浓度使得分离效果不佳。应根据样品实际质量浓度,选择合适检测方法。 |
英文摘要: |
The determination of short-chain fatty acid by ion chromatography and high-performance liquid chromatography(HPLC) was compared from the aspects of separation chromatography, analysis time, linearity range, limit of detection, precision and recovery. HPLC method used SunFireTM C18 chromatography column, mobile phase was KH2PO4 solution and methanol, and flow rate was 1.0 mL/min. Ion chromatography method used DionexTM ATC-3 chromatography column, mobile phase was sodium hydrate solution with different concentrations, and flow rate was 1.5 mL/min. The results showed that analysis time, linearity range, limit of detection, precisions of retention time and peak area, and recovery of HPLC method were 14.5 min, 0-1 200 mg/L, 15.57-23.23 mg/L, 0.079%-0.597%, 1.12%-3.50% and 96.1%-112.0% respectively. For ion chromatography method, they were 13.0 min, 0-20 mg/L, 0.03-0.10 mg/L, 0.000%-0.053%, 1.18%-2.69% and 98.2%-122.0%, respectively. HPLC method had wide detection range, but higher limit of detection. Ion chromatography method had lower limit of detection, but narrow detection range, and higher sampling mass concentration led to poor separation effect. So, the proper detection method should be chosen according to the actual mass concentration of sample. |
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