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Determination of low level nitrite and nitrate in biological, food and environmental samples by gas chromatography-mass spectrometry and liquid chromatography with fluorescence detection

机译:气相色谱-质谱和液相色谱-荧光检测法测定生物,食品和环境样品中的亚硝酸盐和硝酸盐含量低

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Gas chromatography-mass spectrometry (GC-MS) and liquid chromatography with fluorescence detection (LC-FL) methods have been proposed for the determination of low level nitrite and nitrate in biological, food and environmental samples. The methods include derivatization of aqueous nitrite with 2.3-diaminonaphthalene (DAN), enzymatic reduction of nitrate to nitrite, extraction with toluene and chromatographic analyses of highly fluorescent 2,3-naphthotriazole (NAT) derivative of nitrite by using GC-MS in selected-ion-monitoring (SIM) mode and LC-FL Nitrite and nitrate ions in solid samples were extracted with 0.5 M aqueous NaOH by sonication. The recoveries of nitrite and nitrate ions based on CC-MS and LC-FL results were 98.40% and 98.10% and the precision of these methods, as indicated by the relative standard deviations (RSDs) were 1.00% for nitrite and 1.20% for nitrate, respectively. The limits of detection of the GC-MS in SIM mode and LC-FL methods based on S/N = 3 were 0.02 and 0.29 pg/ml for nitrite and 0.03 and 0.30 pg/ml for nitrate, respectively.
机译:有人提出了气相色谱-质谱(GC-MS)和液相色谱-荧光检测(LC-FL)方法来测定生物,食品和环境样品中低含量的亚硝酸盐和硝酸盐的方法。这些方法包括用2.3-二氨基萘(DAN)衍生亚硝酸盐水溶液,将硝酸盐酶催化还原成亚硝酸盐,用甲苯萃取以及通过在选定的色谱柱中使用GC-MS对亚硝酸盐的高荧光2,3-萘三唑(NAT)衍生物进行色谱分析。离子监测(SIM)模式和固体样品中的LC-FL亚硝酸根离子和硝酸根离子用0.5 M NaOH水溶液通过超声提取。根据CC-MS和LC-FL结果,亚硝酸根和硝酸根离子的回收率分别为98.40%和98.10%,这些方法的精密度由亚硝酸根的相对标准偏差(RSD)表示为1.00%,硝酸根的相对标准偏差为1.20%。 , 分别。基于S / N = 3的SIM模式下的GC-MS和LC-FL方法的检测限分别为亚硝酸盐为0.02和0.29 pg / ml,硝酸盐为0.03和0.30 pg / ml。

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