超高效液相色谱-串联质谱法同时测定田螺中3种微囊藻毒素
Simultaneous UHPLC-MS/MS Determination of 3 Microcystic Algae Toxins in Field Snail
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摘要: 采用超高效液相色谱-串联质谱法同时测定田螺中3种微囊藻毒素(微囊藻毒素-RR、微囊藻毒素-LR、微囊藻毒素-YR)的含量。田螺样品经甲醇-水(85+15)混合液提取,Oasis HLB固相萃取柱净化。以UPLC BEH C18色谱柱为固定相,以不同体积比混合的(A)甲酸(0.1+99.9)溶液和(B)甲醇-乙腈(1+1)混合液为流动相做梯度洗脱,采用电喷雾正离子源模式多反应监测检测。3种微囊藻毒素的质量浓度均在1.0~100.0 μg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.05~0.08 μg·kg-1之间。以空白样品为基体进行加标回收试验,所得回收率在67.3%~84.2%之间,相对标准偏差(n=6)在6.1%~8.3%之间。Abstract: UHPLC-MS/MS was applied to the simultaneous determination of 3 microcystic algae toxins (MC-RR, MC-LR and MC-YR ) in field snail. The field snail sample was extracted with methanol (85+15) solution and purified by passing through Oasis HLB-solid phase extraction column. UPLC BEH C18 column was used as stationary phase, and mixtures of (A) formic acid (0.1+99.9) aq. solution and (B) mixture of methanol-acetonitrile (1+1) solution mixed in different ratios were used as mobile phase in gradient elution. ESI+ as well as multi-reactions monitoring was adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 3 microcystic algae toxins were kept in the same range of 1.0-100.0 μg·L-1, with detection limits (3S/N) in the range of 0.05-0.08 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 67.3%-84.2%, with RSD′s (n=6) in the range of 6.1%-8.3%.