QuEChERS前处理结合高效液相色谱法及高效液相色谱-串联质谱法检测葡萄酒中3种赭曲霉毒素
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(1.广东出入境检验检疫局检验检疫技术中心 广东省动植物与食品进出口技术措施研究重点实验室, 广东 广州 510623;2.暨南大学,广东 广州 510010)

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刘青 女 高级工程师 研究方向为食品安全与检测E-mail:gdciqlq@163.com

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国家质检总局科技计划项目(2016IK050)


Detection of three ochratoxins in wine by QuEChERS combined with high performance liquid chromatography and high performance liquid chromatography-tandem mass spectrometry
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(1.Guangdong Key Laboratory of Import and Export Technical Measures of Animal, Plant and Food, Inspection and Quarantine Technology Center of Guangdong Entry-Exit Inspection and Quarantine Bureau, Guangdong Guangzhou 510623, China;2.Jinan University, Guangdong Guangzhou 510010, China)

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    摘要:

    目的 建立QuEChERS净化技术结合高效液相色谱法及高效液相色谱-串联质谱法检测葡萄酒中赭曲霉毒素A(OTA)、赭曲霉毒素B(OTB)和赭曲霉毒素C(OTC)3种赭曲霉毒素的方法。方法 对QuEChERS净化条件和高效液相色谱及高效液相色谱-串联质谱检测条件进行优化,葡萄酒样品先用乙腈-冰乙酸(90∶10,V/V)进行酸化稀释,离心后取上清液经C18+SiO2+MgSO4净化剂组合净化过滤,待测样液经液相色谱C18柱(4.6 mm×250 mm,5 μm)梯度洗脱分离后,分别采用荧光检测器和串联质谱电喷雾技术,在多反应监测(MRM)模式下,实现同时对葡萄酒中OTA、OTB和OTC三种赭曲霉毒素的定性和定量分析。结果 方法最低定量限(LOQ)均为2.0 μg/kg,相对标准偏差(RSD)为2.01%~7.52%(n=6)。结论 该方法操作方便、灵敏度高、重现性好,适用于日常监管工作中对葡萄酒中赭曲霉毒素的检测。

    Abstract:

    Objective Method were developed to detect three ochratoxins including ochratoxin A (OTA), ochratoxin B (OTB) and ochratoxin C (OTC) in wine via QuEChERS combined with high performance liquid chromatography (QuEChERS-HPLC) and HPLC-tandem mass spectrometry (HPLC-MS/MS). Methods The wine samples were diluted with acetonitrile-glacial acetic acid (90∶10, V/V) and then purified with a modified QuEChERS using a scavenging agent combination of C18, SiO2 and MgSO4 after centrifugation. The separation was performed on C18 column (4.6 mm×250 mm, 5 μm) after the gradient elution on a liquid chromatography. Three ochratoxins contaminants in wine were analyzed by HPLC-FLD and HPLC-MS/MS-ESI in the positive ionization under the multiple-reaction monitoring (MRM) mode. Results By these method, the limit of quantification (LOQ) were 2.0 μg/kg and the relative standard deviation (RSD) was between 2.01%-7.52% (n=6). Conclusion The developed methods were proved to be simple, sensitive, reproducible and were suitable for the determination of ochratoxins in wine in daily supervision.

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刘青,庞世琦,熊欣,何素媚,陈文锐,张广文. QuEChERS前处理结合高效液相色谱法及高效液相色谱-串联质谱法检测葡萄酒中3种赭曲霉毒素[J].中国食品卫生杂志,2018,30(5):481-486.

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  • 收稿日期:2018-06-21
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  • 在线发布日期: 2018-09-29
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