TY - JOUR PY - 2013// TI - Determination of paralytic shellfish poisoning toxins by HILIC-MS/MS coupled with dispersive solid phase extraction JO - Food chemistry A1 - Zhuo, Liyang A1 - Yin, Yuechun A1 - Fu, Wusheng A1 - Qiu, Bin A1 - Lin, Zhenyu A1 - Yang, Yiqiang A1 - Zheng, Lemin A1 - Li, Jianrong A1 - Chen, Guonan SP - 115 EP - 121 VL - 137 IS - 1-4 N2 - This paper describes the use of QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) for the extraction, cleanup and detection of 10 paralytic shellfish toxins (PSP) in sea food by HILIC-MS/MS with positive ESI. Matrix matched calibration standards were used to compensate for matrix effects. The toxins were extracted with acetonitrile/water (90:10, v/v) containing 0.1% formic acid and cleaned by HLB and GCB sorbents. Qualitative and quantitative detection for the analytes were carried out under the multiple reaction monitoring (MRM) in positive ionization mode after chromatography separation on a TSK-gel Amide-80® column (150mm×2.0mm×3μm). Studies at three fortification levels for the toxins in the range of 8.1-225.5μg/kg gave mean recoveries from 71.3% to 104.6% with relative standard deviation (RSD)⩽15.8%. The limit of detection (LOD) was below the recommended regulatory limit of 170μgSTX(equ.)/kg and the proposed method fully meets the needs of daily monitoring.

Language: en

LA - en SN - 0308-8146 UR - http://dx.doi.org/10.1016/j.foodchem.2012.10.010 ID - ref1 ER -