超高效液相色谱-串联质谱法检测螺旋藻保健品中7种微囊藻毒素

摘要

采用固相萃取净化结合超高效液相色谱-串联质谱法(UPLC-MS/MS)测定了螺旋藻保健品中7种微囊藻毒素(MCs).螺旋藻保健品经70％(体积分数)的甲醇超声提取,冷冻离心沉淀杂质后,经HLB柱净化.在WatersACQUITY UPLC(R) BEH C18色谱柱上以乙腈和0.2 mmoL/L乙酸铵水溶液为流动相进行梯度洗脱分离,采用电喷雾离子源正离子模式进行多反应离子监测,外标法定量.7种MC在线性范围内线性关系良好(相关系数(r)不小于0.995)；检出限为6.7 ～ 33.3 μg/kg,定量限为20.0～100.0μg/kg.各分析物在阴性螺旋藻保健品中的加标回收率在87.5％～97.9％之间,相对标准偏差(RSD)在1.6％ ～6.9％之间.该方法准确可靠,灵敏度高,可用于螺旋藻保健品中MC污染的确证定性、定量检测.%Ultra performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/ MS) combined with solid phase extraction (SPE) has been developed for the determination of 7 microcystins (MCs) in Spirulina health food products. The sample was extracted by 70% (v/rnv) methanol. The lipid substances were isolated by centrifugation under freezing condition, and then followed by clean-up with a Waters Oasis HLB solid phase extraction cartridge. The separation was performed on a Waters ACQUITY UPLC? BEH C18. column with gradient elution using acetonitrile and 0. 2 mmol/L ammonium acetate. The electrospray ionization ( ESI) source in positive ion mode was used for multiple reaction monitoring (MRM). The external standard method was used for the quantification. The linear ranges for 7 MCs were 20 - 400 p,g/kg, and the correlation coefficients were not less than 0. 995. The limits of detection were 6. 7 - 33. 3 (Jig/kg. The limits of quantification were 20. 0 - 100. 0 jig/kg. The recoveries of the 7 MCs spiked in blank Spirulina samples ranged from 87. 5% to 97. 9% with the relative standard deviations of 1. 6% -6. 9%. The results demonstrated that the method is easy, fast, sensitive, and suitable for the confirmation and quantification of the 7 MCs in Spirulina samples.