离子色谱法测定FAPAS比对肉粉样品中亚硝酸盐、硝酸盐含量

Determination of Nitrite and Nitrate in Meat Powder Samples from Food Analysis Performance Assessment Scheme Using Ion Chromatography with Suppressed Conductivity Detection

为建立离子色谱法测定肉粉样品中亚硝酸盐和硝酸盐含量的方法,将样品经超声和水浴提取后,经阳离子交换树脂柱净化,以氢氧化钾为淋洗液,经Dionex IonPac^(TM)AS19阴离子柱分离,采用AERS 500(4 mm)阴离子抑制器、电导检测器进行检测,标准曲线定量。结果表明:亚硝酸根离子在质量浓度0.10~4.00 mg/L、硝酸根离子在质量浓度0.50~20.00 mg/L范围内线性关系良好,相关系数均为0.999 9;样品中亚硝酸盐和硝酸盐的平均回收率分别为99.53%(n=9)和99.29%(n=9),相对标准偏差分别为0.60%和0.25%。本次比对结果为"满意",表明本方法科学、可靠,适用于基质复杂的熟肉制品中亚硝酸盐和硝酸盐的测定。

This paper is aimed to establish a method for the determination of nitrite and nitrate in meat powder samples from Food Analysis Performance Assessment Scheme （FAPAS） by ion chromatography with suppressed conductivity detection. Samples were extracted ultrasonically in a water bath, and the extract was purified on cation exchange resin column before analysis. The separation was performed on DioneX IonPacTM AS19 anion column with KOH solution as eluent, and the analytes were detected by an AERS 500 （4 ram） anion suppressor and a conductivity detector. The standard curve method was used for quantitative analysis. The linear range of nitrate was from 0.10 to 4.00 mg/L, and the average recovery was 99.53% with a relative standard deviation （RSD） of 0.60% （n = 9）. The linear range of nitrite was from 0,50 to 20.00 mg/L, and the average recovery was 99.29% with a RSD of 0.25% （n = 9）. In addition, both correlation coefficients were 0.999 9. In conclusion, the results of this comparison were satisfactory, and the method was scientific, reliable, and suitable for the determination of nitrite and nitrate in cooked meat products with complex matrix.