阀切换技术-离子色谱法测定水产品中的硼酸盐

建立利用阀切换技术,离子排斥-抑制电导检测器测定水产品中硼酸盐的离子色谱方法。样品经过简单的除蛋白前处理,即可进样分析。采用ICS-1600离子色谱仪(配十通阀),IonPac ICE-Borate离子排斥柱分离,利用阀切换技术,IonPacTBC-1硼酸盐富集柱在线捕获待测成分的同时去除基体干扰,而后进行二次分离。2.5mmol/L MSA+60mmol/L Mannitol作为淋洗液,流速1.0 mL/min,进样量100μL,抑制电导检测。在上述色谱条件下,硼酸的质量浓度在0.1~5.0μg/mL时与色谱峰面积(A)之间的线性关系良好,检出限(S/N=3)为0.02μg/mL。将本方法应用于水产品中硼酸盐的检测,加标回收率为86.5%~93.0%。该方法在线去除基体干扰,简便、快速、准确,可用于实际样品的测定。

Determination of borate in aquatic products by valve-switching ion chromatography

A method was developed for the determination of borate in aquatic products by ICE ion chromatography with valve-switching technology.Sample can be analyzed after simple pretreatment of removing protein.The analytical column was Dionex IonPac ICE-borate(250×9mm),IonPac TBC-1 was used as the concentration column to trap the analytical component and the matrix was excluded at the same time,then the trapped borate was separated once again by valve-switching.2.5mmol/L MSA+ 60mmol/L Mannitol was the eluent at a flow rate of 1.0 mL/min,100μL sample was injected into IC directly,the detection was performed by suppressed conductive detector.The quantitive analysis of external standard calibration curves was used.The linear range of the method was good for the borate in 0.1~5.0μg/mL,and the detection limits(S/N=3) was 0.01μg/mL.The average recovery was 86.5%~93.0%.The method has been applied to determine aquatic products with satisfactory results.