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目的建立在线超滤一离子色谱法检测鱼子酱中多聚磷酸盐的方法。方法利用超纯水超声提取鱼子酱中的多聚磷酸盐,经在线超滤装置自动在线净化样品,由电导检测器检测样品中的多聚磷酸盐含量。结果该方法检出限(LOD)为10 mg/kg。标准加入法测定所有被测物的高、中、低三个浓度加标水平的回收率范围分别为正磷酸盐95%~120%、焦磷酸盐68%~75%、三聚磷酸盐85%~88%、三偏磷酸盐100%~107%,相对标准偏差(RSD)在0.38%~1.36%之间。4种被测物在1~80μg/mL范围内线性良好,R~2均大于0.999。结论该方法稳定、快速、精密度高、线性范围宽,适合鱼子酱中多聚磷酸盐的含量测定。
OBJECTIVE To establish a method for the determination of polyphosphates in caviar by on-line ultrafiltration-ion chromatography. Methods The polyphosphates in caviar were ultrasonically extracted by ultrapure water. The samples were purged online automatically by the on-line ultrafiltration device. The polyphosphate content in the samples was detected by conductance detector. Results The limit of detection (LOD) was 10 mg / kg. The standard addition method for the determination of all tested substances in the high, medium and low spiked levels of the three recovery rates were 95% to 120% orthophosphate, pyrophosphate 68% to 75%, tripolyphosphate 85% ~ 88%, trimetaphosphate 100% ~ 107%, relative standard deviation (RSD) between 0.38% ~ 1.36%. Four kinds of analytes showed good linearity in the range of 1 ~ 80μg / mL with R ~ 2> 0.999. Conclusion The method is stable, rapid, high precision, wide linear range, suitable for determination of polyphosphate in caviar.