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高效液相色谱法快速测定蜂蜜中的微量有机酸

Rapid determination of minority organic acids in honey by high-performance liquid chromatography.

作者信息

Suárez-Luque Silvia, Mato Inés, Huidobro José F, Simal-Lozano Jesús, Sancho M Teresa

机构信息

Facultad de Farmacia, Departamento de Química Analítica, Nutrición y Bromatología, Universidad de Santiago, Santiago de Compostela (Galicia), Spain.

出版信息

J Chromatogr A. 2002 May 10;955(2):207-14. doi: 10.1016/s0021-9673(02)00248-0.

Abstract

A rapid high-performance liquid chromatographic method for the determination of organic acids in honey is reported. Malic, maleic, citric, succinic and fumaric acids were identified and quantified in 15 min. First time repeatibility, reproducibility and recoveries were determined out for these acids in honey samples. Maleic acid was also quantified for first time by a chromatographic method. The organic acids were removed from honey by using a solid-phase extraction procedure with anion-exchange cartridges. Previously, the solution of honey was adjusted to pH 10.50 with 0.1 M NaOH and stirred for 15 min at room temperature. Then, this solution was adjusted to pH 5.00 with 0.1 M H2SO4. This procedure was carried out to avoid interferences in the baseline. The chromatographic separation was achieved with only one Spherisorb ODS-2 S5 column thermostated at 25 degrees C. Metaphosphoric acid (pH 2.20) was used as mobile phase at a flow-rate of 0.7 ml/min. Organic acids were detected with a UV-vis detector (215 nm). The precision results showed that the relative standard deviations of the repeatability and reproducibility were < or =3.20% and < or =4.86%, respectively. The recoveries of the organic acids ranged from 62.9 to 99.4%. Under optimum conditions the detection limits ranged from 0.0064 to 7.57 mg/kg and the quantification limits ranged from 0.025 to 10.93 mg/kg.

摘要

报道了一种快速高效液相色谱法测定蜂蜜中的有机酸。在15分钟内鉴定并定量了苹果酸、马来酸、柠檬酸、琥珀酸和富马酸。首次测定了蜂蜜样品中这些酸的重复性、再现性和回收率。马来酸也首次通过色谱法进行了定量。采用阴离子交换柱固相萃取法从蜂蜜中去除有机酸。此前,用0.1M NaOH将蜂蜜溶液调节至pH 10.50,并在室温下搅拌15分钟。然后,用0.1M H2SO4将该溶液调节至pH 5.00。进行此步骤是为了避免基线干扰。仅使用一根在25℃恒温的Spherisorb ODS-2 S5柱实现色谱分离。以偏磷酸(pH 2.20)为流动相,流速为0.7 ml/min。用紫外可见检测器(215nm)检测有机酸。精密度结果表明,重复性和再现性的相对标准偏差分别≤3.20%和≤4.86%。有机酸的回收率在62.9%至99.4%之间。在最佳条件下,检测限为0.0064至7.57mg/kg,定量限为0.025至10.93mg/kg。

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