1. 广西出入境检验检疫局检验检疫技术中心
2. 广西大学轻工与食品工程学院
3. 上海出入境检验检疫局动植物与食品检验检疫技术中心
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刘晓松, 郑玲, 黄文雯, 等. 浓缩果汁中甲基硫菌灵、2-氨基苯并咪唑、多菌灵、噻菌灵及5-羟基噻菌灵残留量的液相色谱-串联质谱法测定[J]. 分析测试学报, 2013,32(1):84-88.
Simultaneous Determination of Thiophanate-methyl,2-Aminobenzimidazole,Carbendazim,Triabendazole and 5-Hydroxy-triabendazole in Concentrated Fruit Juices by LC-MS/MS[J]. 2013,32(1):84-88.
建立了同时测定浓缩果汁中甲基硫菌灵(TM)、2-氨基苯并咪唑(2-AB)、多菌灵(MBC)、噻菌灵(TBZ)及5-羟基噻菌灵(5-OH-TBZ)的液相色谱-串联质谱法。选取7种代表性浓缩果汁进行研究,果汁样品先用乙腈提取,经PSA柱净化后,用ZORBAX Eclipse XDB-C18柱分离,以10 mmol/L乙酸铵-0.1%甲酸和甲醇为流动相进行梯度洗脱,四极杆串联质谱(MS/MS)采用电喷雾正离子(ESI+)和多反应监测模式(MRM)检测。结果表明:在0.02 ~0.2 mg/L质量浓度范围内各待测物质的线性关系良好,相关系数均不小于0.998 5;2-氨基苯并咪唑和5-羟基噻菌灵的定量下限为2.0 μg/kg,甲基硫菌灵、多菌灵和噻菌灵的定量下限均为1.0 μg/kg。当2-氨基苯并咪唑和5-羟基噻菌灵的加标水平为2、4、20 μg/kg,噻菌灵、多菌灵、甲基硫菌灵的加标水平为1、2、10 μg/kg时,回收率为70%~110%,相对标准偏差为0.1%~10.9%;该方法能有效检测出多种浓缩果汁中此5种杀菌剂及其代谢物的残留量,且稳定性好,结果可靠。
A liquid chromatography tandem mass spectrometric method was developed for the determination of benzimidazole fungicides and their metabolites such as thiophanate-methyl(TM),2-aminobenzimidazole(2-AB),carbendazim(MBC),triabendazole(TBZ),5-hydroxy-triabendazole(5-OH-TBZ) in 7 types of concentrated fruit juices including apple,mango,pineapple,pear,orange,lychee and passion fruit.Seven representative concentrated fruit juices were selected and extracted with acetonitrile.The extracts were purified with PSA column.The separation of 5 analytes was carried out on a ZORBAX Eclipse XDB-C18 column using methanol-10 mmol/L ammonium acetate(containing 0.1% formic acid) as mobile phase by gradient elution.The detection of analytes was performed by electrospray tandem mass spectrometry with ES+ and multiple reaction monitoring (MRM) modes.The results showed that,the method showed good linear relationships in the range of 0.02 -0.2 mg/L for the tested samples,with correlation coefficients no less than 0.998 5.The quantitation limits were 2.0 μg/kg for 2-AB and 5-OH-TBZ,and 1.0 μg/kg for the rest of the analytes.The mean recoveries ranged from 70% to 110% with relative standard deviations of 0.1%-10.9% when the fortified levels for 2-AB and 5-OH-TBZ were 2,4,20 μg/kg and those for TBZ,MBC,TM were 1,2,10 μg/kg,respectively.The proposed method was sensitive and reliable,and was successfully applied in the determination of benzimidazole fungicides and their metabolites in real commercial concentrated juices.
LC-MS/MS浓缩果汁甲基硫菌灵2-氨基苯并咪唑多菌灵噻菌灵5-羟基噻菌灵
liquid chromatography tandem mass spectrometryconcentrated fruit juicesthiophanate-methyl2-aminobenzimidazolecarbendazimtriabendazole5-hydroxy-triabendazole
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