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目的:建立河豚鱼肝中河豚毒素(TTX)的亲水液相色谱-三重四极杆质谱联用(LC-MS-MS)定量检测方法。方法:样品经匀浆,超声,乙腈沉淀离心后,取上清液进样测定。极性聚酰胺键合硅胶柱InnovationTMHP Amide(100 mm×3.0mm,5μm),流动相乙腈-0.3%甲酸(体积比为70∶30),流速为0.5 mL·min-1;柱温30℃,进样量5μL。选择正离子多反应监测(MRM)模式,[M+H]+,m/z 320.1162.1进行定量分析。结果:TTX的线性范围为0.031 3～2.00 mg·L-1(r=0.999 9);检测限(S/N=3)为3.0 pg,加样回收率在96.3%～103.0%。结论:该法灵敏度高,重复性好,简便快速,适用于河豚毒素的测定。
Objective: To establish a quantitative liquid chromatography-triple quadrupole mass spectrometry (LC-MS-MS) method for the determination of tetrodotoxin (TTX) in liver of puffer fish. Methods: After the sample was homogenized, sonicated and centrifuged by acetonitrile, the supernatant was taken for injection. The polar polyamide bonded silica gel column InnovationTM HP Amide (100 mm × 3.0 mm, 5 μm), mobile phase of acetonitrile-0.3% formic acid (volume ratio of 70:30), the flow rate of 0.5 mL · min- Injection volume 5μL. Positive ion multiple reaction monitoring (MRM) mode was selected, [M + H] +, m / z 320.1162.1 for quantitative analysis. Results: The linear range of TTX was 0.031 3 ~ 2.00 mg · L-1 (r = 0.999 9). The detection limit (S / N = 3) was 3.0 pg and the recoveries ranged from 96.3% to 103.0%. Conclusion: The method has high sensitivity, good repeatability, simple and rapid, suitable for the determination of tetrodotoxin.