动物源性食品中硝基酚钠残留量的测定

Determination of Sodium Nitrophenolate Residues in Animal Products

建立一种固相萃取-超高效液相色谱串联质谱分析新方法,用于动物源性食品中硝基酚钠3种残留组分(5-硝基邻甲氧基苯酚钠、邻硝基苯酚钠和对硝基苯酚钠)的定量检测。样品经乙腈超声提取,阴离子固相萃取柱(MAX)净化,经C18色谱柱分离,用超高效液相色谱串联质谱检测。该方法中对硝基苯酚钠、5-硝基邻甲氧基苯酚钠和邻硝基苯酚钠的检出限分别为0.5, 0.5和50μg/kg,线性范围为0.5~1 000μg/L,其线性系数均大于0.999;实际样品中对硝基酚钠、5-硝基邻甲氧基苯酚钠在0.5, 1.0和5.0μg/kg,邻硝基酚钠在50, 100和500μg/kg 3个不同添加水平的回收率分别为75.3%~93.9%, 71.9%~93.6%和64.1%~91.1%,相对标准偏差分别为3.3%~14%, 3.3%~15%和2.8%~15%。该方法快速简便,灵敏度较高,精密度较好,可用于动物源性食品中硝基酚钠残留量的检测。

A new solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) method was developed for the determination of three residual components of sodium nitrophenolate(5-nitroguaiacol sodium, 2-nitrophenol sodium and 4-nitrophenol sodium) in animal products. The samples were first subject to ultrasonic extraction with the acetonitrile as solvent. Then the products were purified by anion solid phase extraction(MAX), followed by the separation and detection by UPLC-MS/MS equipped with a C18 chromatography column. The limits of detection of 4-nitrophenol sodium, 5-nitroguaiacol sodium and 2-nitrophenol sodium were 0.5 μg/kg, 0.5 μg/kg and 50 μg/kg, respectively.The linear ranges were 0.5-1 000 μg/L. The linear correlation coefficients were >0.999. The recoveries of 4-nitrophenol sodium, 5-nitroguaiacol sodium and 2-nitrophenol sodium in animal products at three different levels(0.5, 1.0 and 5.0 μg/kg for 4-nitrophenol sodium and 5-nitroguaiacol sodium, 50, 100 and 500 μg/kg for 2-nitrophenol sodium) were 75.3%-93.9%,71.9%-93.6% and 64.1%-91.1%, respectively. The relative standard deviations were 3.3%-14%, 3.3%-15% and 2.8%-15%.With rapid response, high sensitivity and high precision, this method was promising for the determination of sodium nitrophenolate in animal products.