Zhong Yingying, Chen Ping, Yu Xuejun, Xu Diming, Fang Keteng, Peng Jinfeng
Technical Center of Ningbo Entry-Exit Inspection and Quarantine Bureau, Ningbo 315012, China.
Se Pu. 2012 Jun;30(6):635-40. doi: 10.3724/sp.j.1123.2011.12086.
Nitrite and nitrate are common inorganic salts in the diet and drinking water. It is generally believed that excessive intake of these substances may result in methemoglobinemia or other diseases. However, the traditional detection methods for nitrite and nitrate in dairy products restrain their applications to routine analysis due to the presence of certain limitations. In order to solve this problem, an improved national food safety standard method for the determination of nitrite and nitrate in dairy products has been studied. After water extraction, protein precipitation and centrifugation, the supernatant was cleaned up by a solid phase extraction (SPE) column. The eluent mainly composed of sodium hydroxide with acetonitrile as organic modifier. External water mode was used for suppressor. An AS 19 column was used as the analytical column, and the oven temperature was 30 degrees C while the cell temperature was 35 degrees C. The detection wavelength was 225 nm and the injection volume was 200 microL. The results showed that good linearity existed when the concentrations of nitrite and nitrate were between 0.005 -0.50 and 0.05 - 1.50 mg/L respectively. The detection limits of nitrite and nitrate were 0.2 and 0.04 mg/kg respectively when using a conductivity detector; while the values were only 0.02 and 0.01 mg/kg using an ultraviolet (UV) detector. The recoveries were between 84.0% and 104.1% when analyzing dairy products. It is a simple, fast and highly sensitive way for nitrite and nitrate detections.
亚硝酸盐和硝酸盐是饮食和饮用水中常见的无机盐。一般认为,过量摄入这些物质可能导致高铁血红蛋白血症或其他疾病。然而,由于存在某些局限性,乳制品中亚硝酸盐和硝酸盐的传统检测方法限制了它们在常规分析中的应用。为了解决这个问题,研究了一种改进的国家食品安全标准方法来测定乳制品中的亚硝酸盐和硝酸盐。经过水提取、蛋白质沉淀和离心后,上清液通过固相萃取(SPE)柱进行净化。洗脱液主要由氢氧化钠组成,以乙腈作为有机改性剂。采用外加水模式作为抑制器。使用AS 19柱作为分析柱,柱温为30℃,池温为35℃。检测波长为225nm,进样体积为200μL。结果表明,亚硝酸盐和硝酸盐浓度分别在0.005 - 0.50和0.05 - 1.50mg/L之间时具有良好的线性关系。使用电导检测器时,亚硝酸盐和硝酸盐的检出限分别为0.2和0.04mg/kg;而使用紫外(UV)检测器时,该值仅为0.02和0.01mg/kg。分析乳制品时回收率在84.0%至104.1%之间。这是一种用于亚硝酸盐和硝酸盐检测的简单、快速且高度灵敏的方法。