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阴离子交换色谱-积分脉冲安培检测法测定牛奶中硫氰酸钠

Determination of Sodium Thiocyanate in Milk by Anion Exchange Chromatography with Integrated Pulsed Amperometric Detection

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【作者】 卢春黄振中

【Author】 LU Chun;HUANG Zhen-zhong;Jiangxi Nanchang Teachers College;College of Chemistry and Chemical Engineering,Jiangxi Normal University;

【机构】 南昌师范高等专科学校江西师范大学化学化工学院

【摘要】 建立了牛奶中硫氰酸钠的离子色谱-积分脉冲安培检测器分析方法。样品用无水乙醇提取,经ENVI-18固相萃取小柱净化,采用IonPac?AG21保护柱(2×50mm)和IonPac?AS21分析柱(2×250mm)分离,积分脉冲安培检测器检测。在1.0mg/kg和5.0mg/kg两个水平添加时的平均回收率(n=5)分别为92.4%和105%,相对标准偏差分别为9.94%和6.79%。方法最低检出限为0.20mg/kg(S/N=3),用于实际牛奶样品中硫氰酸钠测定,结果满意。

【Abstract】 A new method for analysis of sodium thiocyanate in milk was proposed.Sodium thiocyanate was extracted from milk samples with anhydrous ethanol and cleaned-up by ENVI-18SPE column.The target analyte was separated on a Dionex IonPac AS21(2×250mm)analytical column and IonPac?AG21(2×50 mm)guard column with 25mM sodium hydroxide,and detected by integrated pulsed amperometric detection(IPAD)using an Au working electrode in combination with a pH-Ag/AgCl reference electrode in AgCl mode.The mean recoveries at the spike level of 1.0and 5.0mg/kg were 92.4%and 105% with relative standard deviations of 9.94% and 6.79%,respectively.The limit of detection of the method was 0.20mg/kg(S/N=3).Satisfactory results were obtained in the determination of sodium thiocyanate in milk samples.

  • 【分类号】O657.1;TS252.7
  • 【被引频次】1
  • 【下载频次】73
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