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首页> 外文期刊>Journal of separation science. >Simultaneous determination of 13 carbohydrates using high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry
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Simultaneous determination of 13 carbohydrates using high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry

机译:使用高性能阴离子交换色谱法同时测定13个碳水化合物,耦合脉冲倍流检测和质谱法

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摘要

A simple, accurate, and highly sensitive method was developed for the determination of 13 carbohydrates in polysaccharide of Spirulina platensis based on high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry. Samples were extracted with deionized water using ultrasonic-assisted extraction, and the ultrasound-assisted extraction conditions were optimized by Box-Behnken design. Then the extracted polysaccharide was hydrolyzed by adding 1 mol/L trifluoroacetic acid before determination by high-performance anion-exchange chromatography coupled with pulsed amperometric detection and confirmed by high-performance anion-exchange chromatography coupled with mass spectrometry. The high-performance anion-exchange chromatography coupled with pulsed amperometric detection method was performed on a CarboPac PA20 column by gradient elution using deionized water, 0.1 mol/L sodium hydroxide solution, and 0.4 mol/L sodium acetate solution. Excellent linearity was observed in the range of 0.05-10 mg/L. The average recoveries ranged from 80.7 to 121.7%. The limits of detection and limits of quantification for 13 carbohydrates were 0.02-0.10 and 0.2-1.2 mu g/kg, respectively. The developed method has been successfully applied to ambient samples, and the results indicated that high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry could provide a rapid and accurate method for the simultaneous determination of carbohydrates.
机译:基于高性能阴离子 - 交换色谱法与脉冲电流检测和质谱法测定螺旋藻铂的多糖中的13种碳水化合物,开发了一种简单,准确和高度敏感的方法。使用超声波辅助提取用去离子水提取样品,通过Box-Behnken设计优化了超声辅助提取条件。然后通过加入1mol / L三氟乙酸在用高性能阴离子 - 交换色谱法测定之前加入萃取的多糖水解,并通过高性能阴离子 - 交换色谱和质谱法耦合的高性能阴离子交换色谱法证实。通过使用去离子水,0.1mol / L氢氧化钠溶液和0.4mol / L乙酸钠溶液,通过梯度洗脱对碳波PA20柱进行高性能阴离子交换色谱法。在0.05-10mg / L的范围内观察到优异的线性度。平均回收率范围为80.7至121.7%。 13个碳水化合物的定量限制分别为0.02-0.10和0.2-1.2μg/ kg。已经成功地应用于环境样品的开发方法,结果表明,与脉冲电流检测和质谱相偶联的高性能阴离子交换色谱法可以提供一种快速和准确的方法,用于同时测定碳水化合物。

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