食品科学 ›› 2019, Vol. 40 ›› Issue (10): 304-310.doi: 10.7506/spkx1002-6630-20180509-141

• 安全检测 • 上一篇    下一篇

QuEChERS-高效液相色谱-串联质谱测定牛奶中6种玉米赤霉烯酮类毒素

谢瑜杰1,2,陈 辉2,彭 涛2,*,代汉慧2,胡雪艳2,范春林2,呼秀智1,薛占永1,*   

  1. 1.河北工程大学生命科学与食品工程学院,河北 邯郸 056021;2.中国检验检疫科学研究院,北京 100176
  • 出版日期:2019-05-25 发布日期:2019-05-31
  • 基金资助:
    国家科技基础性工作专项(2013FY113100);“十三五”国家重点研发计划重点专项(2017YFF0211301)

Determination of Six Zeranols in Milk by QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

XIE Yujie1,2, CHEN Hui2, PENG Tao2,*, DAI Hanhui2, HU Xueyan2, FAN Chunlin2, HU Xiuzhi1, XUE Zhanyong1,*   

  1. 1. College of Life Science and Food Engineering, Hebei University of Engineering, Handan 056021, China; 2. Chinese Academy of Inspection and Quarantine, Beijing 100176, China
  • Online:2019-05-25 Published:2019-05-31

摘要: 建立QuEChERS-高效液相色谱-串联质谱同时检测牛奶中6 种玉米赤霉烯酮类毒素残留量的检测方法。样品用1%乙酸-乙腈提取,乙腈饱和正己烷除脂,C18、N-丙基乙二胺和无水硫酸镁净化,在ZORBAX SB-C18色谱柱上分离,以5 mmol/L NH4Ac溶液和乙腈作为流动相进行梯度洗脱,电喷雾离子源负离子模式扫描,多反应监测测定,基质匹配外标法定量分析。牛奶中6 种玉米赤霉烯酮类毒素在0.1~50 μg/L质量浓度范围内呈线性关系,相关系数均高于0.995;检出限为0.05~0.1 μg/kg,定量限为0.25~0.5 μg/kg。牛奶中6 种玉米赤霉烯酮类毒素的3 个加标水平的平均回收率范围为91.8%~114.5%,相对标准偏差在3.2%~14.4%之间(n=6)。

关键词: 玉米赤霉烯酮类毒素, QuEChERS, 高效液相色谱-串联质谱, 牛奶

Abstract: A method for simultaneous determination of six zeranols residues in milk was developed by quick, easy cheap, effective, rugged and safe (QuEChERS) extraction coupled to high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was extracted with 1% acetate acetonitrile. The extract was degreased with acetonitrile-saturated n-hexane, cleaned up with a mixture of C18, primary secondary amine (PSA) and magnesium sulfate anhydrous. The analytes were separated on a reversed phase C18 column and gradiently eluted with 5 mmol/L ammonium acetate and acetonitrile. These analytes were analyzed under the multiple reaction monitoring (MRM) mode with negative electrospray ionization (ESI-) and quantified by matrix-matched external standard method. Good linearity was obtained for the six zeranols in the concentration range of 0.1–50 μg/L with correlation coefficients of more than 0.995. The limits of detection (LODs) and the limits of quantification (LOQs) for the zeranols were 0.05–0.1 and 0.25–0.5 μg/kg, respectively. The recoveries at three spiked concentration levels were in the range of 91.8%–114.5%. The repeatability expressed as relative standard deviation (RSD) ranged from 3.2% to 14.4% (n = 6).

Key words: zeranols, QuEChERS, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), milk

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