| 液相色谱-串联质谱法测定葡萄酒中赭曲霉毒素A |
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| 引用本文： | 侯建波,;谢文,;李杰,;沈炜锋,;何建敏.液相色谱-串联质谱法测定葡萄酒中赭曲霉毒素A[J].中国酿造,2014(5):146-149. |
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| 作者姓名： | 侯建波 ;谢文 ;李杰 ;沈炜锋 ;何建敏 |
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| 作者单位： | [1]浙江出入境检验检疫局技术中心,浙江杭州310016; [2]浙江省检验检疫科学技术研究院,浙江杭州310016; [3]浙江立德产品技术有限公司,浙江杭州310016 |
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| 基金项目： | 浙江省重点科技创新团队项目（2010R50028）;质检总局科技计划项目（2013IK188） |
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| 摘 要： | 以赭曲霉毒素B为内标物,建立了应用固相萃取-液相色谱-串联质谱法(SPE-LC-MS/MS)对葡萄酒中赭曲霉毒素A残留量测定的方法。葡萄酒样品经过调节pH值至7.0和C18固相萃取净化的前处理过程后,采用液相色谱-串联质谱法进行测定(正离子方式,多反应监测模式)。方法定量限(LOQ)为2.0g/L。内标法定量计算,在0~10g/L质量浓度范围内线性相关系数0.998。在葡萄酒中分别进行2.0g/L、4.0g/L和8.0g/L三个添加水平的测试,该检测方法回收率范围97.6%~109.7%,相对标准偏差(RSD)3.0%~4.6%。方法简便、快速、准确,可用于葡萄酒中赭曲霉毒素A的定量测定。
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| 关 键 词： | 葡萄酒 赭曲霉毒素A 内标法 液相色谱-串联质谱法 |
Determination of ochratoxin A in wine by LC-MS/MS |
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| Affiliation: | HOU Jianbo, XIE Wen, LI Jie, SHEN Weifeng, HE Jianmin (1.Zhejiang Entry-exit Inspection and Quarantine Bureau, Hangzhnu 310016, China; 2.Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou 310016, China, 3.Zhejiang Lead Product Technic Co., Ltd., Hangzhou 310016, China) |
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| Abstract: | Using ochratoxin B as internal standard substance, the application of SPE-LC-MS/MS for determination of ochratoxin A in wine sample was established. The sample was adjusted to pH 7.0 and purified with C18 solid phase extraction pretreatment process. The quantitative detection was carried out by LC-MS/MS, using a positive-ion electrospray ionization in multiple reaction monitoring mode, and the limits of quantification was 2.0 g/L. The working curves were linear in the range of 0-10 g/L, and the correlation coefficients were more than 0.998. Ochratoxin A addition in 2.0 g/L, 4.0 g/L and 8.0 g/L levels was added and the recovery rate ranged from 97.6% to 109.7% with relative standard deviations between 3.0% and 4.6%. This method was simple, rapid, accurate and adapted to confirm residues of ochratoxin A in wine. |
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| Keywords: | wine ochratoxin A internal standard method LC-MS/MS |
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