Conductance detection of nitrate and nitrite in livestock and poultrymuscle by inhibitory ion chromatography
SUN Yanqin1,2,3, ZHANG Fangfang4, SHEN Juan1,2,3, WU Xinyi1,2,3, LI Chunbao1,2,3, CHEN Ying5, WANG Wei1,2,3*
1(College of Food Science and Technology, Nanjing Agricultural University, Nanjing 210095, China) 2(National Center of Meat Quality and Safety Control, Nanjing Agricultural University, Nanjing 210095, China) 3(Supervision, Inspection and Testing Center for Quality of Meat-Products(Nanjing), Ministry of Agricultureand Rural Affairs, Nanjing Agricultural University, Nanjing 210095, China) 4(Thermo Fisher Scientific, Shanghai 201206, China) 5(China Institute of Inspection and Quarantine Science, Beijing 100176, China)
摘要 在优化前处理方法和仪器检测条件的基础上,建立了一种可同时检测畜禽肉及其制品中硝酸盐和亚硝酸盐含量的抑制型离子色谱法(inhibitory ion chromatography)。样品均质后,经超声萃取、静置分离,加入二氯甲烷除去蛋白质、脂肪等物质。取上清液过滤净化,以KOH为淋洗液,采用抑制型离子色谱法电导检测器检测。硝酸盐与亚硝酸盐的分离度良好,定量限分别为0.3、0.2 mg/kg,检出限分别为0.09、0.06 mg/kg,并分别在0.2~2.0、0.02~0.2 mg/kg浓度内,呈良好线性关系。在低、中、高3个浓度水平加标并平行测定6次,猪、牛、羊、鸡和鸭中硝酸盐和亚硝酸盐的加标回收率平均值分别在77.0%~106.1%、77.3%~101.0%、65%~97.5%、80.0%~103.3%、90.5%~99.2%,平均相对标准偏差(relative standard diviation, RSD)均<8.75%。该研究建立的方法简便快捷,检测结果准确可靠、回收率高、精密度良好,可以满足畜禽肉及其制品中硝酸盐与亚硝酸盐的同时检测。
Abstract: Based on the optimized pretreatment method and instrument detection conditions, an inhibitory ion chromatography method was established to simultaneously detect the contents of nitrate and nitrite in livestock, poultry and their products. The samples were homogenized, extracted by ultrasound, and then separated by static separation. After removing protein, fat, and other substances by dichloromethane extraction, the supernatant was filtered and purified. And then the purified samples were analyzed by ion chromatography (IC) using KOH solution as eluent and detected by a suppressed conductivity detector. The results showed that the separation degree of nitrate and nitrite was good, the quantitation limit were 0.3 and 0.2 mg/kg and the detection limit were 0.09 and 0.06 mg/kg. Nitrate and nitrite showed good linear relationship in the range of 0.2-2.0 mg/kg and 0.02-0.2 mg/kg, respectively. Three concentration levels, low, medium and high, were labeled and measured six times in parallel. The average nominal recovery rates of nitrate and nitrite in pig, cattle, sheep, chicken and duck were between 77.0%-106.1%, 77.3%-101.0%, 65%-97.5%, 80.0%-103.3% and 90.5%-99.2%, respectively. And the average relative standard deviation (RSD) was less than 8.75%. The method established in this study is simple and fast, with accurate and reliable and can be used for simultaneous detection of nitrate and nitrite in livestock, poultry and their products.
孙延勤,张芳芳,沈娟,等. 抑制型离子色谱法电导检测畜禽肉中硝酸盐和亚硝酸盐[J]. 食品与发酵工业, 2020, 46(11): 264-268.
SUN Yanqin,ZHANG Fangfang,SHEN Juan,et al. Conductance detection of nitrate and nitrite in livestock and poultrymuscle by inhibitory ion chromatography[J]. Food and Fermentation Industries, 2020, 46(11): 264-268.