超高效液相色谱-串联质谱法测定多脂肪类 动物源性食品中硝基呋喃代谢物
目的 建立多脂肪类动物源性样品中4种硝基呋喃代谢物的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)的快速检测方法。方法 样品利用硅藻土充分研磨后, 增加0.125 mol/L盐酸用量至25 mL进行衍生, 调节pH值后, 使用32 mL提取溶剂乙酸乙酯, 分2次提取, 提取溶剂合并旋干后, 加入定容试剂, 超声提取1.5 min, 加入2.5 mL正己烷提取脂肪, 水相过滤上机检测。分析物采用电喷雾电离, 正离子扫描, 多反应检测模式(multiple reaction monitoring, MRM), 基质匹配内标标准曲线法定量。结果 4种代谢物的工作曲线在0.5~30.0 μg/L浓度范围内线性良好, 相关系数r2均达到了0.998以上, 5-吗啉甲基-3-氨基-2-恶唑烷基酮(3-amino-5-morpholinomethyl-2-oxazolidinone, AMOZ)、1-氨基-乙内酰脲(1-amino-hydantoin, AHD)、3-氨基-2-恶唑酮(3-amino-2-oxalidinone, AOZ)、氨基脲(semicarbazide, SEM)最低检出限分别为0.052、0.043、0.049、0.108 μg/kg。平均回收率在84.5%~105.4%之间, 相对标准偏差1.26%~7.58%。结论 方法解决了多脂类动物源性样品中硝基呋喃代谢物易干扰、回收低、检不准的难点, 同时使用4种硝基呋喃代谢物内标定量结果, 结果准确可靠、适用多脂肪类样品中硝基呋喃代谢物的检测。
Objective To establish a analytical method for detection of metabolites of nitrofuran in fatty animal samples by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The derivatives of samples were generated in 25 mL hydrochloric acid (0.125 mol/L) and extracted by 32 mL ethyl acetate after being grinded with diatomaceous earth. Before extraction of fat, nitrofuran metabolites in pear-shaped bottle were extracted by ultrasonic about 1.5 min. Identification was achieved by electrospray ionization in positive mode (ESI+) using multiple reaction monitoring (MRM). Results The calibration curves of the 4 analytes showed a good linearity in the concentrations of 0.5-30 μg/L with r2 above 0.998. The limits of detection of 3-amino-5-morpholinomethyl-2-oxazolidinone (AMOZ), 1-amino-hydantoin (AHD), 3-amino-2-oxalidinone (AOZ), and semicarbazide (SEM) were 0.052, 0.043, 0.049, and 0.108 μg/kg, respectively. The average recoveries were 84.5%-105.4% with relative standard deviations (RSDs) of 1.26%-7.58%. Conclusion This method solves the difficulties of easy interference, low recovery and inaccuracy of fatty animal samples of nitrofuran metabolites, and is accurate and reliable with internal standard, which can be applied for detection of fatty animal samples of nitrofuran metabolites.
标题：超高效液相色谱-串联质谱法测定多脂肪类 动物源性食品中硝基呋喃代谢物
英文标题：Determination of metabolites of nitrofuran in fatty animal samples by ultra performance liquid chromatography-tandem mass spectrometry
作者：
高洁 济宁出入境检验检疫局
朱莉萍 济宁出入境检验检疫局
倪永付 济宁出入境检验检疫局
田晓林 济宁出入境检验检疫局
李修平 济宁出入境检验检疫局
中文关键词:硝基呋喃代谢物,超高效液相色谱-串联质谱法,硅藻土,多脂类动物源性样品,
英文关键词:nitrofuran metabolites,ultra performance liquid chromatography-tandem mass spectrometry,diatomaceous earth,fatty animal samples,
发表日期：2018-01-02
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