实时直接分析-串联质谱法测定葡萄酒中赭曲霉毒素A

色谱 , 2017, 35(2): 185-190. doi: 10.3724/SP.J.1123.2016.07008

实时直接分析-串联质谱法测定葡萄酒中赭曲霉毒素A

宫小明 ^1, , 马荣桧 ^2, , 王洪涛 ^3, , 郭礼强 ^4, , 李凯 ^5, , 吴振兴 ^6, , 赵晗 ^7, , 孙军 ^8,

1.潍坊出入境检验检疫局,山东潍坊,261041

2.潍坊出入境检验检疫局,山东潍坊,261041

3.潍坊出入境检验检疫局,山东潍坊,261041

4.潍坊出入境检验检疫局,山东潍坊,261041

5.潍坊出入境检验检疫局,山东潍坊,261041

6.山东出入境检验检疫局检验检疫技术中心,山东青岛,266002

7.潍坊出入境检验检疫局,山东潍坊,261041

8.潍坊出入境检验检疫局,山东潍坊,261041

基金项目: 国家质检总局科研基金资助项目(2013IK177).Scientific Research Fund Project of General Administration of Quality Supervision and Inspection and Quarantine of the Peoples Republic of China (2013IK177)

关键词： QuEChERS , 同位素稀释内标 , 实时直接进样分析 , 串联质谱法 , 赭曲霉毒素A , 葡萄酒

Determination of ochratoxin A in wine by direct analysis in real time-tandem mass spectrometry

Keywords： QuEChERS , isotope dilution internal standard , direct analysis in real time (DART) , tandem mass spectrometry (MS/MS) , ochratoxin A (OTA) , wine

建立了葡萄酒中赭曲霉毒素A的实时直接分析-串联质谱(DART-MS/MS)方法.前处理采用乙酸乙酯提取,二甲基十八碳硅烷粉(ODS)粉分散固相萃取净化,采用DART-MS/MS检测,同位素稀释内标法定量.结果表明:在1.0、2.0、10 μg/kg3个加标水平下,回收率为88.7％～ 105.7％,RSD为8.5％～ 12.8％,定量限为0.5 μg/kg.该方法具有简单、快速、灵敏度高等特点,能满足葡萄酒中赭曲霉毒素A检测的要求.

A method for the determination of ochratoxin A (OTA) in wine was developed using direct analysis in real time-electrospray ionization tandem mass spectrometry (DART-MS/MS).The sample was extracted with ethyl acetate and purified by votexing with ODS powder,detected using DART-MS/MS.The results showed that the average recoveries ranged from 88.7％ to 105.7％ with the RSDs of 8.5％-12.8％ at three spiked levels of 1.0,2.0,and 10 μg/kg.The LOQ was 0.5 μg/kg.The proposed method was accurate,rapid and reliable,which can be successfully applied to the qualitative and quantitative analysis of ochratoxin A in wine.

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