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目的建立水产品中3种麻痹性贝类毒素成分(GTX2,3、dcSTX和STX)的柱前荧光衍生高效液相色谱(HPLC-FLD)检测方法。方法样品用1%乙酸提取,C18固相萃取柱净化,2%H2O2荧光衍生,以Symmetry?C18柱(4.6mm×150mm,5μm)为色谱柱分离,以乙腈和0.1mol/L甲酸铵(595)作为流动相,流速1.0mL/min,荧光检测器激发波长340nm,发射波长395nm。结果该法在10~500μg/L范围内线性关系良好,平均加标回收率为72.5%~88.6%,RSD为2.8%~4.7%。方法的检出限分别为dcSTX 3μg/kg、STX 10μg/kg和GTX2,34μg/kg。结论本方法灵敏度高、结果可靠,为检测水产品贝类麻痹性毒素的含量提供了一种高效便捷的方法。
Objective To establish a pre-column fluorescence-based high performance liquid chromatography (HPLC-FLD) method for the determination of three paralytic shellfish toxins (GTX2,3, dcSTX and STX) in aquatic products. Methods The samples were extracted with 1% acetic acid, purified with a C18 solid phase extraction cartridge and derivatized with 2% H2O2. The chromatographic separation was performed on a Symmetry C18 column (4.6 mm × 150 mm, 5 μm) using acetonitrile and 0.1 mol / L ammonium formate 95) as the mobile phase, flow rate 1.0mL / min, fluorescence detector excitation wavelength 340nm, emission wavelength 395nm. Results The method showed a good linearity in the range of 10 ~ 500 μg / L. The average recoveries were 72.5% ~ 88.6% with RSDs of 2.8% ~ 4.7%. The detection limits of the method were dcSTX 3μg / kg, STX 10μg / kg and GTX2, 34μg / kg respectively. Conclusion The method has high sensitivity and reliable results, and provides an efficient and convenient method for the determination of shellfish paralytic toxins in aquatic products.