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  

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

作　　者：钟志雄[1] 李攻科[2] 

机构地区：[1]广东省疾病预防控制中心,广东广州510300 [2]中山大学化学与化学工程学院,广东广州510275

出　　处：《色谱》2009年第4期499-504,共6页Chinese Journal of Chromatography

基　　金：广东省医学科研基金项目(A2006079)

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100mmol/LNaOH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0.3～60mg/L,检出限为2.1～2.3mg/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。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 mmx 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.

关 键 词：离子色谱法 磷酸盐 焦磷酸盐 偏磷酸盐 总磷 海产品 

分 类 号：O658[理学—分析化学]