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背景:失忆性贝毒属于海洋神经毒素,是一类具有神经兴奋的氨基酸类物质,其主要成分为软骨藻酸。贝类通过滤食毒藻,将软骨藻酸富集在体内,人类因食用被软骨藻类污染的贝类而中毒。目的:建立液相色谱/四极杆-行时间质谱联用技术对贝类样品中的软骨藻酸实施有效监控,以期提高贝类的食用安全性。设计:前瞻性自身对照实验。单位:上海检验检疫局动植物与食品检验检疫技术中心理化实验室。材料:MUS-1B贻贝组织标样[(36±1)μg软骨藻酸/g,批号MUS-1B0159]和软骨藻酸标准溶液(100mg/L,批号软骨藻类CS-1C352)购自NationalResearchCouncilofCanada(Halifax,Canada)。实际贻贝样品取自历年在东海爆发的赤潮海域收集得到的阳性贝类,空白样品购自市集。高效液相色谱仪(Waters2695)配有紫外检测器(Waters2487)和四极杆-飞行时间质谱仪(QUltima,Micromass)。方法:样品用甲醇-水(体积比为1∶1)提取,经SAX固相萃取柱净化后,用ZorbaxEclipseXDB-18柱(250×2.1mm,3.5μm)色谱分离,流动相为乙腈/水含0.05%甲酸,梯度淋洗,流速0.20mL/min。四极杆-飞行时间质谱选择电喷雾正离子模式,以[M+H]+作为前体离子进行飞行时间质谱扫描测定。主要观察指标:①检测限。②液相色谱/四极杆-飞行时间质谱法的准确度与精密度。结果:样品加标的平
BACKGROUND: Amnesia shellfish belong to marine neurotoxin, which is a class of amino acids with nervous excitability. Its main component is domoic acid. Shellfish poisoning algae by filtration, the accumulation of domoic acid in the body, humans due to consumption of chondroitin contaminated shellfish and poisoning. Objective: To establish a liquid chromatography / quadrupole-line time-of-flight mass spectrometry technique for the effective monitoring of domoic acid in shellfish samples in order to improve the food safety of shellfish. Design: Prospective self-control experiment. Unit: Physical and Chemical Laboratory of Animal and Plant Inspection and Quarantine Technology Center, Shanghai Inspection and Quarantine Bureau. MATERIALS: MUS-1B Mussel Tissue Standards [(36 ± 1) μg Domoic Acid / g, Lot MUS-1B0159] and Domoic Acid Standards (100 mg / L, Lot Chondroitin CS-1C352) were purchased from National Research Council of Canada Halifax, Canada). The actual mussel samples were taken from positive shellfish collected in the red tide waters that broke out in the East China Sea in previous years. Blank samples were purchased from the market. High performance liquid chromatography (Waters 2695) equipped with a UV detector (Waters 2487) and a quadrupole-time-of-flight mass spectrometer (QUltima, Micromass). Methods: The sample was extracted with methanol-water (1: 1 by volume), purified by SAX solid-phase extraction cartridge and chromatographed on a Zorbax Eclipse XDB-18 column (250 × 2.1 mm, 3.5 μm) 0.05% formic acid, gradient elution, flow rate 0.20 mL / min. Quadrupole-TOF mass spectrometry Electrospray positive ion mode was selected and time-of-flight mass spectrometry was performed using [M + H] + as precursor ion. The main observation indicators: ① detection limit. ② liquid chromatography / quadrupole - time of flight mass spectrometry accuracy and precision. Results: Sample spiked flat