超高效液相色谱-串联质谱法检测熟肉制品中10种工业染料残留
目的 建立超高效液相色谱—串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定熟肉制品中10种工业染料的检测方法。方法 熟肉制品样品均质后经乙腈、乙腈水溶液(1:1, V:V)分别提取后, 采用冷冻离心处理去除提取液中油脂及天然大分子色素。采用ACQUITY UPLC BEH C18色谱柱分离后, 用UPLC-MS/MS于电喷雾正离子源和多反应监测扫描模式下测定10种工业染料, 基质匹配标准曲线结合稳定同位素内标法定量。结果 10种目标化合物阴性加标水平在2、5、10 ?g/kg下, 回收率为68.5%~91.3%, 相对标准偏差为2.4% ~12.8%。10种目标化合物的检出限为0.05~0.7 ?g/kg, 定量限为0.15 ~2.0 ?g/kg。用该方法对30件熟牛肉、熟猪肝、烤肠、香肠等样品进行了目标化合物的检测, 未检测到工业染料残留。结论 该方法操作简便、快速, 灵敏度和准确度高, 包含种类较宽, 具有一定的拓展性, 可为熟肉制品中工业染料残留的日常监控提供更方便、快捷的检测方法支持。
Objective To establish an analytical method for determination of 10 industrial dyes residues in cooked meat products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After homogenization, cooked samples were extracted with acetonitrile and acetonitrile-water (1:1, V:V), and then the oil and natural macromolecular pigment in the extraction solution were removed by freezing and centrifuging. The separation was performed on ACQUITY UPLC BEH C18 column, then the 10 industrial dyes were detected by UPLC-MS/MS with ESI positive ion scan (ESI+) in mode of multiple reaction monitoring (MRM) and quantified by matrix standard curve combined with stable isotope internal standard method for quantification. Results At the spiked level of 2, 5 and 10 ?g/kg, the recoveries of each compound were in the range of 68.5%–91.3% with the relative standard deviation of 2.4%–12.8%. The limits of detection were 0.05–0.7 ?g/kg and the limits of quantitative were 0.15–2.0 ?g/kg for the 10 targets compounds. This method was used to detect the target compounds in 30 samples of cooked beef, cooked pig liver, baked sausage and sausage so on, and no industrial dye residue was detected. Conclusion The proposed method is simple, fast, sensitive and accurate, with a wide variety and a certain development. It can provide a more convenient and fast detection method for daily monitoring of industrial dye residues in cooked meat products.
标题:超高效液相色谱-串联质谱法检测熟肉制品中10种工业染料残留
英文标题:Determination of 10 industrial dyes in cooked meat products by ultra performance liquid chromatography-tandem mass spectrometry
作者:
范赛 北京市疾病预防控制中心,北京市预防医学研究中心,食物中毒诊断溯源技术北京市重点实验室
张楠 北京市疾病预防控制中心,北京市预防医学研究中心,食物中毒诊断溯源技术北京市重点实验室
刘平 北京市疾病预防控制中心,北京市预防医学研究中心,食物中毒诊断溯源技术北京市重点实验室
王莉莉 北京市疾病预防控制中心,北京市预防医学研究中心,食物中毒诊断溯源技术北京市重点实验室
吴国华 北京市疾病预防控制中心,北京市预防医学研究中心,食物中毒诊断溯源技术北京市重点实验室
赵榕 北京市疾病预防控制中心,北京市预防医学研究中心,食物中毒诊断溯源技术北京市重点实验室
中文关键词:工业染料,超高效液相色谱-串联质谱法,熟肉制品,残留,
英文关键词:industrial dye,ultra performance liquid chromatography-tandem mass spectrometry,cooked meat products,residues,
发表日期:2020-04-13
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