咖啡中3种赭曲霉毒素QuEChERS-UPLC-MS/MS检测方法
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(海南省食品检验检测中心国家市场监管重点实验室〔热带果蔬质量与安全〕,海南 海口 570100)

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高云慨,男,海南省食品检验检测中心中级工程师,硕士。

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尹青春(1986—),女,海南省食品检验检测中心高级工程师,硕士。E-mail: yinqingchun@163.com

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国家市场监管重点实验室(热带果蔬质量与安全)自主研究课题(编号:ZZ-2022001)


Establishment of QuEChERS-UPLC-MS/MS method to determine three kinds of ochratoxins in coffee
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(Hainan Institute for Food Control, Key Laboratory of Tropical Fruits and Vegetables Quality Safety for State Market Regulation, Haikou, Hainan 570100, China)

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    摘要:

    目的:建立同时测定咖啡中3种赭曲霉毒素的QuEChERS-超高效液相色谱—串联质谱检测方法。方法:样品经乙腈—水—甲酸(V乙腈VV甲酸为55∶40∶5)超声提取,利用QuEChERS盐包进行脱水盐析,过ZanChERS-Myco17净化小柱净化。样品采用0.2%甲酸水—乙腈作为流动相经Waters BEH C18(1.7 μm,2.1 mm×100 mm)色谱柱梯度洗脱分离。电喷雾正离子模式,多反应监测扫描,内标法定量。结果:3种目标物在0.1~20.0 ng/mL的质量浓度范围内线性关系良好,相关系数≥0.999 46,方法检出限和定量限分别为0.1~0.2,0.2~0.7 μg/kg。咖啡基质中3个添加水平目标物平均回收率为79.0%~103.3%,相对标准偏差为1.5%~7.6%。结论:该方法前处理简单,重现性好,分析时间短,能够适用于不同咖啡基质样品中3种赭曲霉毒素残留的高通量检测。

    Abstract:

    Objective: A new method was developed for the simultaneous determination of three kinds of ochratoxins in coffee by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with QuEChERS pretreatment. Methods: Samples were extracted by acetonitri-water-formic acid solution (55∶40∶5) with ultrasonic, salted out with a QuEChERS salt pocket, and then purified with a (ZanChERS-Myco17) column. The chromatographic separation was performed on an ACQUITY UPLC BEH C18 (1.7 μm, 2.1 mm×100 mm) column by gradient elution using a mobile phase comprising 0.2% formic acid aqueous solution and acetonitrile. In the positive ion mode of electric spray, the samples detected were used by multiple reaction monitoring (MRM) modes with internal standard method. Results: Three target substances had a good linear relationship in the range of 0.1~20.0 ng/mL, and the correlation coefficient was greater than 0.999 46. The detection limit and quantitative limit were 0.1~0.2 μg/kg and 0.2~0.7 μg/kg, respectively. Average recoveries at three spiked levels in the coffee matrix were 79.0%~103.3% with a relative standard deviation of 1.5%~7.6%. Conclusion: This method has the advantages of simple sample pretreatment, good reproducibility and high efficiency, and is suitable for the high-throughput detection of multiple ochratoxins in different coffee samples.

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高云慨,陈小妹,陈春泉,等.咖啡中3种赭曲霉毒素QuEChERS-UPLC-MS/MS检测方法[J].食品与机械,2023,39(11):91-97.
GAO Yunkai, CHEN Xiaomei, CHEN Chunqian, et al. Establishment of QuEChERS-UPLC-MS/MS method to determine three kinds of ochratoxins in coffee[J]. Food & Machinery,2023,39(11):91-97.

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  • 收稿日期:2023-02-09
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  • 在线发布日期: 2023-12-26
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