首页> 中文期刊> 《色谱》 >超高效液相色谱法同时测定香精香料中14种禁限用物质

超高效液相色谱法同时测定香精香料中14种禁限用物质

         

摘要

A high performance liquid chromatographic (HPLC) method has been developed for the simultaneous determination of meso-erythritol and L-erythrulose in fermentation broth. The chromatographic conditions were as follows: Lichrospher 5-NH2 column (250 mm × 4. 6 mm) with the temperature of 30 ℃ , acetonitrile-water (90= 10, v/v) as mobile phase with the flow rate of 1. 0 mL/min. meso-Erythritol was detected by refractive index (RI) detector at 35 ℃ and L-erythrulose was detected by ultraviolet (UV) detector at 277 nm at room temperature. The linear range for meso-erythritol was 1.00 - 100.00 g/L with a correlation coefficient of 0. 998 5. The limit of detection (LOD) and the limit of quantification (LOQ) for meso-erythritol were 0. 10 g/L and 0. 45 g/L, respectively. The linear range for L-erythrulose was 1. 00 - 100. 00 g/L with a correlation coefficient of 0. 995 8. The LOD and LOQ for L-erythrulose were 0. 50 g/L and 0. 87 g/L, respectively. The relative standard deviations (RSDs) of intraday and interday for meso-erythritol were less than 3. 28% and 5. 30%, respectively. The intraday and interday RSDs for L-erythrulose were less than 2. 16% and 2. 25%, respectively. The recoveries of meso-erythritol and L-erythrulose in fermentation broth were greater than 99%. The samples from fermentation broth were detected at different time points. The measurement by the novel HPLC method was not affected by the other components in the fermentation broth. Furthermore, the HPLC method can be used for the determination of the substrate meso-erythritol and the product L-erythrulose simultaneously.%建立了超高效液相色谱-二极管阵列检测器( UPLC-PDA)同时测定香精香料中14种禁限用物质的方法.样品经10% (v/v)甲醇水溶液(含1% (v/v)氨水)提取后进行UPLC测定.采用的色谱柱为Waters BEH C18柱(50mm×2.1 mm,1.7μm),流动相为10 mmol/L乙酸铵(含0.1%乙酸)和乙腈,梯度洗脱,流速为0.2 mL/min,柱温为35℃,在200~ 500 nm范围内进行扫描检测.结果表明,该方法在12 min内可实现14种禁限用物质的分离和检测,在0.10~ 50 mg/L范围内具有较好的线性关系,各待测物的线性相关系数均大于0.995,检出限(以信噪比为3计)为0.32~2.51 mg/kg.在5、10、20 mg/L添加水平下待测物的平均回收率为93.0% ~121.0%,相对标准偏差为0.51%~4.50%.该方法操作简易,灵敏度高,线性相关性好,重复性佳,可以满足国内对于香精香料样品中禁限用物质的检测要求.

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