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建立了对西加鱼毒素中主要成分P-CTX-1的高效液相色谱质谱联用检测方法。色谱条件为色谱柱C18(2.1mm×50mm,1.7μm),柱温40℃。以0.1%甲酸-5mmol/L乙酸铵水溶液和乙腈溶液作为流动相,梯度洗脱(0～3.0min50%A→5%A,3.0～4.5min5%A→50%A),流速为0.6mL/min。质谱条件为电喷雾正离子模式,[M+NH4]+作为前体离子进行多级反应监测,以质荷比(m/z)为1058和1076的子离子分别作为P-CTX-1的定性和定量离子,源温度105℃,喷雾温度350℃,提取电压4.0V,锥气流速49mL/min,喷雾气流速750L/h。在此检测条件下西加鱼毒素P-CTX-1的检出限达0.175μg/L,平均加标回收率为66.0±2.0%,相对标准偏差为6.0%。利用该方法检测了6份采自西太平洋珊瑚礁的鱼类样品,在其中5份样品中检测出P-CTX-1。
A high-performance liquid chromatography-mass spectrometry (LC-MS / MS) method was established for the determination of P-CTX-1, a major component of Xijia fish toxin. The chromatographic conditions were column C18 (2.1 mm × 50 mm, 1.7 μm) and the column temperature was 40 ° C. The mobile phase consisted of a gradient of 0.1% formic acid in 5 mmol / L ammonium acetate and acetonitrile (0-3.0min50% A → 5% A, 3.0-4.5min5% A → 50% A) at a flow rate of0.6mL / min. Mass spectrometry conditions were electrospray positive ion mode and [M + NH4] + was used as a precursor ion for multistage reaction monitoring. Qualities of P-CTX-1 with daughter ions of mass-to-charge ratio (m / z) of 1058 and 1076 respectively The ionization temperature was 105 ℃, the temperature was 350 ℃, the extraction voltage was 4.0V, the flow rate of conical gas was 49mL / min and the flow rate of spray gas was 750L / h. Under this condition, the detection limit of P-CTX-1 was 0.175μg / L, the average recovery was 66.0 ± 2.0% and the relative standard deviation was 6.0%. Six fish samples collected from the Western Pacific coral reefs were detected using this method and P-CTX-1 was detected in five of the samples.