Zhong Zhixiong, Li Gongke
Center for Disease Control and Prevention of Guangdong Province, Guangzhou, China.
Se Pu. 2009 Jul;27(4):499-504.
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 x 4 mm) and an IonPac AG11-HC guard column (50 mm x 4 mm) using 30 - 80 mmol/L KOH gradient elution at a flow rate of 1.0 mL/min at 35 degrees C, 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.
建立了一种用离子色谱法(IC)测定海产品中磷酸盐、焦磷酸盐、偏磷酸盐和总磷的方法。测定磷酸盐、焦磷酸盐、偏磷酸盐的样品在室温下用100 mmol/L氢氧化钠溶液提取;测定总磷的样品经高温灰化消解;然后用固相萃取(SPE)柱消除干扰。采用IonPac AS11-HC分析柱(250 mm×4 mm)和IonPac AG11-HC保护柱(50 mm×4 mm)进行分离,在35℃下以1.0 mL/min的流速用30 - 80 mmol/L氢氧化钾梯度洗脱,配备抑制型电导检测器。在最佳条件下,20分钟内可完成测定。考察了pH值、有机溶剂和共存离子的影响。线性范围为0.3 - 60 mg/L,检出限为2.1 mg/kg至2.3 mg/kg,相对标准偏差为1.6%至2.6%。该方法用于鱼虾中阴离子的测定,回收率为81.8% - 100.0%。该方法具有高选择性、高灵敏度,对实际样品分析结果令人满意。