离子色谱法测定燕窝中的多聚磷酸盐

Determination of polyphosphates in bird’s nest by ion chromatography

中文关键词:  离子色谱  燕窝  多聚磷酸盐

英文关键词:ion chromatography  bird’s nest  polyphosphates

中文摘要:

      目的 利用离子色谱(IC)建立一种可以一次进样同时分离测定燕窝中的正磷酸盐、焦磷酸盐、三聚磷酸盐和三偏磷酸盐的分析方法。方法 将燕窝磨成粗粉, 经超声萃取, 再用氯仿沉淀蛋白, 过C18柱后采用AS11-HC离子色谱柱(4 mm?250 mm), 流动相为NaOH和超纯水, 梯度洗脱, 流速为1.0 mL/min, 电导抑制检测。结果 该方法在0.5~100 mg/L范围内有良好的线性关系, 相关系数均大于0.9996,在添加实验中, 方法的回收率在89.5%~106.3%之间 ,相对标准偏差为0.9%~7.3%。正磷酸盐、焦磷酸盐、三聚磷酸盐和三偏磷酸盐的检测限分别为0.2、0.05、0.05、0.1 mg/kg。结论 该方法检测限低, 灵敏度和重现性高, 抗干扰能力强, 结果准确, 操作方便快速, 适合燕窝中多聚磷酸盐的测定。

英文摘要:

      Objective An ion chromatography (IC) method was developed for simultaneous determination of orthophosphate，pyrophosphate，tripolyphosphate and trimetaphosphate in bird’s nest. Methods Bird’s nest was milled into powder, and the protein in Bird’s nest was precipitated by chloroform after ultrasonic extraction. The extracts were cleaned-up by C18 SPE cartridge, then separated by AS11-HC (4 mm ? 250 mm) column, used NaOH and ultrapure water as the mobile phase, gradient elution with the flow rate of 1 mL/min, finally detected by conductivity inhibit detection. Results The linear range of the method was 0.5~100 mg/L with R2>0.9996.The average recoveries of spiked samples were between 89.5% to 106.3% with the relative standard deviations (RSD) of 0.9%~7.3%.The limit of detections (LODs) were 0.2, 0.05, 0.05 and 0.1 mg/kg for orthophosphate, pyrophosphate, tripolyphosphate and trimetaphosphate, respectively. Conclusion The proposed method is rapid, sensitive and accurate for the deter-mination of polyphosphates in the bird's nest.