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通过超声提取、固相萃取纯化、超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF-MS)联用技术快速测定水产品中的微囊藻毒素-RR、-YR、-LR和节球藻毒素。分别采用选择离子监测质荷比(m/z)为519.84、1045.66、995.67、825.54分子离子峰进行定量分析。该法检出限为5.0～10.0μg/kg,在浓度0.02～5 mg/kg的范围内,峰面积与样品浓度呈良好线性关系;4种藻毒素的回收率为76.2%～93.7%,相对标准偏差为2.0%～7.1%。采用上述方法对45个太湖水产品样品进行测定,发现有少量水产品中存在藻毒素污染,其中微囊藻毒素-RR最高含量为15.2μg/kg,微囊藻毒素-LR最高含量为0.84μg/kg,MC-YR、节球藻毒素均未检出。此方法可作为监测水产品体内蓄积藻毒素的分析方法。
Rapid determination of microcystin-LR, -YR, aquatic products in aquatic products by ultrasonic extraction, SPE-SPE and UPLC-Q-TOF- -LR and Synutoxin. Selected ions were used to monitor the mass-to-charge ratio (m / z) for the 519.84,1045.66,995.67,825.54 molecular ion peak quantitative analysis. The detection limit of the method was 5.0 ~ 10.0μg / kg. The linear range of the peak area was within the range of 0.02 ~ 5 mg / kg. The recoveries of the four phytotoxins ranged from 76.2% to 93.7% The standard deviation of 2.0% to 7.1%. Using the above method, 45 samples of Taihu aquatic products were determined and found to be contaminated with algal toxins in a small amount of aquatic products. The maximum content of microcystin-RR was 15.2μg / kg and the maximum content of microcystin-LR was 0.84μg / kg, MC-YR, nodulated algae were not detected. This method can be used as an analytical method for monitoring the accumulation of algal toxins in aquatic products.