超高效液相色谱-三重四极杆串联质谱法测定双壳类水产品中亲脂性贝类毒素

Determination of lipophilic phycotoxins in bivalves aquatic products by ultra performance liquid chromatography coupled with triple quadrupole mass spectrometry

中文关键词:  双壳类  亲脂性贝类毒素  高效液相色谱-三重四极杆串联质谱法  固相萃取

英文关键词:bivalves  lipophilic phycotoxins  ultra performance liquid chromatography coupled with triple quadrupole mass spectrometry  solid phase extraction

中文摘要:

      目的 建立超高效液相色谱-三重四极杆串联质谱法(high performance liquid chromatography coupled with triple quadrupole mass spectrometry, HPLC-TQ-MS/MS)方法检测双壳类水产中的亲脂性贝类毒素(lipophilicphycotoxins, LPs)。方法 样品采用80%甲醇水溶液进行提取, 上清液经strata-x柱净化, 将洗脱液氮吹至干定容后上机测定。选用Agilent ZORBAX Eclipse Plus C18(2.1 mm×50 mm, 1.8 μm)色谱柱, 以10 mmol/L甲酸铵-0.1%甲酸水和乙腈(含0.1%甲酸)为流动相, 采用梯度洗脱进行分离。多重态反应监测(multiple reaction monitoring, MRM)方式检测。结果 LPs的线性范围为5.0~200 ng/mL, 检出限为5.0~6.0 μg/kg, 回收率在45.8%~86.3%之间。结论 本方法提取效果较好、基质效应小, 适用于双壳类水产中亲脂性贝类毒素的痕量检测。

英文摘要:

      Objective To establish a method for determination of lipophilicphycotoxins (LPs) in bivalves aquatic products by ultra performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-TQ-MS/MS). Methods LPs was extracted by 80% methanol solution, and supernatant was loaded on strata-x cartridge. The eluent was dried up by nitrogen blowing, then detected by UPLC-TQ-MS/MS. The sample was separated on an Agilent ZORBAX Eclipse Plus C18 (2.1 mm×50 mm, 1.8 μm) column with water contained 10 mmol/L ammonium formate-0.1% formic acid and acetonitrile contained 0.1% formic acid as mobile phase with gradient elution. The detection was carried out by multiple reaction monitoring (MRM). Results LPs had a good linear in the range of 5.0~200 ng/mL. The limits of detection were 5.0~6.0 μg/kg in bivalves aquatic products, and the recoveries were 45.8%~86.3%. Conclusion This method has good effect of extraction and low matrix inhibition effect, which is suitable for trace detection of lipophilic phycotoxins in bivalves aquatic products.