离子色谱法测定牛奶及奶制品中硝酸盐和亚硝酸盐  

Determination of Nitrate and Nitrite in Milk and Dairy Products by Ion Chromatography

作　　者：邹沫君 ZOU Mojun(Leshan Center for Food and Drug Control,Leshan 614000)

机构地区：[1]乐山市食品药品检验检测中心,乐山614000

出　　处：《食品工业》2023年第7期304-308,共5页The Food Industry

摘　　要：建立离子色谱/电导检测法测定牛奶及奶制品中硝酸盐和亚硝酸盐残留量的分析方法。试样经乙腈-水(4∶6,V∶V)溶液沉淀蛋白,在提取温度75℃,超声提取30 min条件下,经固相萃取小柱净化。选用IonPac AS 19阴离子交换分离柱,在线产生6~70 mmol/L KOH淋洗液梯度洗脱,采用抑制型电导检测器检测硝酸盐与亚硝酸盐。硝酸盐的线性范围0.0~2.0 mg/L,相关系数0.9999,试样在3个不同水平(0.25,0.5和2.5 mg/kg)下的加标回收率为92.98%~104.53%,SRSD值为0.91%~1.23%,检出限为0.075 mg/kg,定量限为0.25 mg/kg。亚硝酸盐的线性范围0.0~0.20 mg/L,相关系数0.9999,试样在3个不同水平(0.12,0.24和1.20 mg/kg)下的加标回收率为92.85%~105.50%,SRSD值为0.86%~1.21%,检出限为0.05 mg/kg,定量限为0.17 mg/kg。该方法操作简便、提取速度快、定性定量准确、灵敏度高,适合牛奶及奶制品中硝酸盐和亚硝酸盐残留量的检测。A new method was established to determine nitrate and nitrite in milk and dairy products by ion chromatography with conducting detection.The protein was precipitated from the sample in acetonitrile and water(4∶6,V/V),and then purified through solid phase extraction columns under the conditions of extraction temperature of 75℃and ultrasonic extraction for 30 min.The separation was performed on an Dionex IonPac AS 19 anion analytical column.Gradient elution using 6-70 mmol/LKOH aqueous solution as the mobile phase was performed,and nitrate and nitrite were detected by ion chromatography.The linear range of nitrate nitrogen was 0.0-2.0 mg/L,the correlation coefficient r was 0.9999,the recoveries(standard additive concentration was 0.25,0.5 and 2.5 mg/kg)were in the range of 92.98%-104.53%,the SRSD was in the range of 0.91%-1.23%,the detection limit was 0.075 mg/kg,and the quantitative limit was 0.25 mg/kg.The linear range of nitrite nitrogen was 0.0-0.20 mg/L,the correlation coefficient r was 0.9999,the recoveries(standard additive concentration was 0.12,0.24 and 1.20 mg/kg)were in the range of 92.85%-105.50%,the SRSD was in the range of 0.86%-1.21%,the detection limit was 0.05 mg/kg,and the quantitative limit was 0.17 mg/kg.This method was easy to operate,fast to extract,accurate and suitable for the detection of nitrate and nitrite in milk and dairy products.

关 键 词：硝酸盐 亚硝酸盐 离子色谱法 牛奶及奶制品 电导检测 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程] O657.7[轻工技术与工程—食品科学与工程]