超高效液相色谱-串联质谱法同步测定贝类水产品中4种脂溶性藻毒素
超高效液相色谱-串联质谱法同步测定贝类水产品中4种脂溶性藻毒素
目的建立一种超高效液相色谱-串联质谱法同时测定贝类产品中4种脂溶性藻毒的方法。方法样品采用甲醇均质提取, 用HLB小柱净化, 在乙腈-5 mmol/L醋酸铵水溶液体系中, 经Kinetex C18柱(150 mm×3 mm, 2.6 μm)梯度洗脱, 实现了4种藻毒素的良好分离。采用了电喷雾正负离子同时监测模式对4种脂溶性藻毒素进行外标法定量测定。结果目标化合物的检出限为2.3～20.7 pg/g, 在3.8～1378.0 pg/g浓度范围内线性良好, 相关系数r2在0.99407~0.99923之间, 同时以贝类产品为基底的4种化合物在高、中、低3个加标水平浓度下的回收率为70%~95%, 相对标准偏差(relative standard deviation, RSD)为2.3%~7.7%。结论该方法灵敏、准确、高效, 适合用于贝类水产品食用安全的日常风险监测项目中。
ObjectiveTo establish a method for simultaneous determination of 4 kinds of lipophilic algae toxins in shellfish products using ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). MethodsSamples were first extracted by methanol, followed by a purification using an Oasis HLB SPE column. Further separation of the 4 targets compound was achieved on a Kinetex C18 column (150 mm×3 mm, 2.6 μm) via UPLC by gradient elution with acetonitrile and 5 mmol/L ammonium acetate aqueous solutionas mobile phase. Quantification of the 4 targets was performed on a mass spectrometry, which simultaneously carried out by means of electrospray ionization in positive (ESI＋) and negative ion mode (ESI-) mode with an external standard. ResultsThe method showed a good linearity in the concentration range of 3.81378.0 pg/g, with the detection limits of 2.320.7 pg/g. The correlation coefficients (r2) were between 0.994070.99923 for 4 toxins. The average recoveries for the high, medium and low concentrations of external standard were between 70%95% with the relative standard deviations(RSD) 2.3%7.7%. ConclusionThe method is sensitive, accurate, with high efficiency and is suitable for the daily risk monitoring project of shellfish food safety.
标题：超高效液相色谱-串联质谱法同步测定贝类水产品中4种脂溶性藻毒素
英文标题：Simultaneous determination of 4 types of lipophilic algae toxins in shellfish products using ultra performance liquid chromatography tandem mass spectrometry
作者：
黄碧慧 厦门市食品药品质量检验研究院
中文关键词:超高效液相色谱-串联质谱法,贝类产品,脂溶性藻毒素,电喷雾电离,正负离子模式,同时监测,
英文关键词:ultra performance liquid chromatography tandem mass spectrometry,shellfish products,lipophilic algae toxins,electrospray ionization,positive and negative ion mode,simultaneous determination,
发表日期：2019-11-20
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