食品科学 ›› 2020, Vol. 41 ›› Issue (18): 311-316.doi: 10.7506/spkx1002-6630-20190617-171

• 安全检测 • 上一篇    

二维超高效液相色谱-三重四极杆/复合线性离子阱质谱联用法快速测定水产品及其制品中河豚毒素

张秀尧,蔡欣欣,张晓艺,李瑞芬   

  1. (温州市疾病预防控制中心,浙江?温州 325001)
  • 出版日期:2020-09-25 发布日期:2020-09-18

Rapid Determination of Tetrodotoxin in Fresh and Processed Aquatic Products by Two-Dimensional Ultra-high Performance Liquid Chromatography-Triple Quadrupole/Linear Ion Trap Mass Spectrometry

ZHANG Xiuyao, CAI Xinxin, ZHANG Xiaoyi, LI Ruifen   

  1. (Wenzhou Municipal Center for Disease Control and Prevention, Wenzhou 325001, China)
  • Online:2020-09-25 Published:2020-09-18

摘要: 建立中心切割二维超高效液相色谱-三重四极杆/复合线性离子阱质谱联用法快速测定水产品及其制品中河豚毒素的方法。样品经0.2%乙酸溶液提取,提取液用0.2%乙酸溶液稀释和过滤后直接进样分析。使用2 种不同性质固定相的色谱柱(Hypercarb PGC和Acquity BEH Amide)通过二位六通切换阀连接,样品先经第1维起反相色谱分离作用的多孔石墨碳色谱柱Hypercarb PGC(2.1?mm×100?mm,3?μm)分离,再将分离出含有河豚毒素的流分切割至捕集柱XBridge BEH Amide guard column(起亲水色谱分离作用的酰胺色谱柱)(4.6?mm×10?mm,2.5?μm)中进行捕集,然后再将捕集柱切换至第2维的流路中,洗入第2维起亲水色谱分离作用的酰胺色谱柱Acquity BEH Amide(2.1?mm×100?mm,1.7?μm)中进行分离,电喷雾正离子模式多离子监测触发的增强子离子扫描方式检测,溶剂标准外标法定量。水产品中河豚毒素的平均加标回收率为82.3%~95.4%,相对标准偏差在2.1%~14%之间(n=6),方法的定量限(RSN=10)为0.002?mg/kg。本法操作简单、灵敏度高、选择性好,可应用于水产品及其制品中河豚毒素的检测。

关键词: 河豚毒素;水产品及其制品;中心切割;二维超高效液相色谱-三重四极杆/复合线性离子阱质谱

Abstract: In this study, a heart-cutting two-dimensional ultra-high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry method was developed and successfully validated for the determination of tetrodotoxin (TTX) in fresh and processed aquatic products. This method was based on the use of two different stationary phase columns (Hypercarb PGC and Acquity BEH Amide), which were connected through a six-port two-position switching valve. Samples were extracted with 0.2% (V/V) acetic acid aqueous solution, and then the extract was diluted with the solvent, filtered and directly injected for analysis. The separation of TTX was carried out on a Hypercarb PGC (2.1 mm × 100 mm, 3 μm) as the 1st dimension through elution with 0.2% (V/V) formic acid aqueous solution. The fraction containing TTX was switched into a trap column (XBridge BEH Amide guard column (4.6?mm × 10?mm, 2.5?μm)), and acetonitrile was simultaneously merged into the fraction by a dilution pump through a tee. After the trap column retained the TTX completely, the valve switched it into the 2nd dimensional stream, and then the TTX was separated on an Acquity BEH Amide (2.1 mm × 100 mm, 1.7 μm) with gradient elution using acetonitrile-H2O both containing 0.1% (V/V) formic acid, detected by positive electrospray ionization tandem mass spectrometry in the multiple reaction monitoring information-dependent acquisition enhanced product ion scanning (MRM-IDA-EPI) mode, and quantified by standard solvent external standard method. The average spiked recoveries were 82.3%–95.4% with relative standard deviations (RSDs) of 2.1%–14% (n = 6). The limit of quantitation (RSN = 10) was 0.002 mg/kg. This simple, selective and sensitive method has been successfully applied to the determination of TTX in fresh and processed aquatic products.

Key words: tetrodotoxin; fresh and processed aquatic products; heart-cutting; two-dimensional ultra-high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry

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