title: Determination of paralytic shellfish poisoning toxins by HILIC-MS/MS coupled with dispersive solid phase extraction.
abstract: 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 (150 mm×2.0 mm×3 μm). Studies at three fortification levels for the toxins in the range of 8.1-225.5 μg/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 170 μgSTX(equ.)/kg and the proposed method fully meets the needs of daily monitoring.
authors.affiliation: Ministry of Education Key Laboratory of Analysis and Detection Technology for Food Safety-Fuzhou University, Fujian Province Key Laboratory of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou 350002, China.
authors.forename: Liyang
authors.initials: L
authors.lastname: Zhuo
authors.forename: Yuechun
authors.initials: Y
authors.lastname: Yin
authors.forename: Wusheng
authors.initials: W
authors.lastname: Fu
authors.forename: Bin
authors.initials: B
authors.lastname: Qiu
authors.forename: Zhenyu
authors.initials: Z
authors.lastname: Lin
authors.forename: Yiqiang
authors.initials: Y
authors.lastname: Yang
authors.forename: Lemin
authors.initials: L
authors.lastname: Zheng
authors.forename: Jianrong
authors.initials: J
authors.lastname: Li
authors.forename: Guonan
authors.initials: G
authors.lastname: Chen
mesh_terms: D002851:Chromatography, High Pressure Liquid; D005506:Food Contamination / Q000032:analysis*; D006801:Humans; D008387:Marine Toxins / Q000032:analysis* / Q000302:isolation & purification*; D017747:Seafood / Q000032:analysis*; D057096:Shellfish Poisoning / Q000175:diagnosis; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D008387:Marine Toxins