色谱

色谱

• 研究论文 • 上一篇    下一篇

离子色谱法测定海产品中磷酸盐、焦磷酸盐、偏磷酸盐和总磷

钟志雄1*, 李攻科2   

  1. 1.Center for Disease Control and Prevention of Guangdong Province, Guangzhou 510300, China; 2.School of Chemistry and Chemical Engineering, Sun Yat-Sen University, Guangzhou 510275, China
  • 收稿日期:2008-12-08 修回日期:2009-02-09 出版日期:2009-07-30 发布日期:1982-06-25
  • 通讯作者: 钟志雄

Determination of phosphate, pyrophosphate, metaphosphate and total phosphorus in seafoods by ion chromatography

ZHONG Zhixiong1*, LI Gongke2   

  1. 1.Center for Disease Control and Prevention of Guangdong Province, Guangzhou 510300, China; 2.School of Chemistry and Chemical Engineering, Sun Yat-Sen University, Guangzhou 510275, China
  • Received:2008-12-08 Revised:2009-02-09 Online:2009-07-30 Published:1982-06-25
  • Contact: ZHONG Zhixiong

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923

被引次数

36

摘要： 建立了离子色谱法测定海产品中磷酸盐、焦磷酸盐、偏磷酸盐和总磷的分析方法。样品经100 mmol/L NaOH溶液浸提,固相萃取柱去除有机物、阳离子、中和OH~后用于海产品中磷酸盐、焦磷酸盐和偏磷酸盐的测定;样品经干灰化法消化,固相萃取柱净化后用于总磷测定。考察了提取溶液的pH、有机物和共存离子对测定结果的影响。该方法的线性范围为0.3～60 mg/L,检出限为2.1～2.3 mg/kg,相对标准偏差为1.6%～2.6%。海鱼和虾仁样品中目标物的加标回收率为81.8%～100.0%。该方法选择性好,灵敏度高,用于实际样品测定结果令人满意。

关键词: 海产品 , 焦磷酸盐, 离子色谱法, 磷酸盐, 偏磷酸盐, 总磷

Abstract: A method for the determination of phosphate, pyrophosphate, metaphosphate and total phosphorus in seafoods by ion chromatography (IC) was developed. The samples for the determination of phosphate, pyrophosphate, metaphosphate were extracted by 100 mmol/L NaOH solution at room temperature; the samples for the determination of total phosphorus were digested by incineration at high temperature; and then solid phase extraction (SPE) column was used to eliminate the interferences. The separation was carried out on an IonPac AS11-HC analytical column (250 mm×4 mm) and an IonPac AG11-HC guard column (50 mm×4 mm) using 30~80 mmol/L KOH gradient elution at a flow rate of 1.0 mL/min at 35 ℃, coupled with a suppressor-type conductivity detector. Under optimum conditions, the measurement could be completed within 20 min. The effects of pH value, organic solvent and coexisted ions were investigated. The linear range was 0.3~60 mg/L, the detection limits were from 2.1 mg/kg to 2.3 mg/kg, and the relative standard deviations were from 1.6% to 2.6%. The method was applied to the determination of anions in fish and shrimps with the recoveries of 81.8%~100.0%. The method offered high selectivity, sensitivity, and gave a satisfactory results for real sample analysis.

Key words: metaphosphate, phosphate, pyrophosphate, seafoods , total phosphorus, ion chromatography (IC)