超高效液相色谱-串联质谱法快速测定地表水中9种藻毒素

Rapid Determination of 9Algal Toxins in Surface Water by UHPLC-MS/MS

采用超高效液相色谱-串联质谱法快速测定地表水中9种藻毒素的含量。地表水样经滤网过滤,离心后,所得上清液以Waters Acquity BEH130色谱柱为分离柱,以不同体积比的0.1%(体积分数,下同)甲酸溶液和含0.1%甲酸的乙腈的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾正离子源和多反应监测模式。9种藻毒素的质量浓度在一定范围内与其对应的峰面积呈线性关系,方法的检出限为0.084～0.175μg·L^(-1)。以空白样品为基体进行加标回收试验,所得回收率为79.4%～113%,测定值的相对标准偏差(n=7)为5.1%～14%。

UHPLC-MS/MS was applied to the rapid determination of 9 algal toxins in surface water. The surface water sample was filtered by strainer. After centrifugation, the supernatant was obtained. Waters Acquity BEH130 chromatographic column was used as stationary phase, and the mixture of 0.1% （φ, the same below） formic acid solution and acetonitrile （containing 0.1% formic acid） mixed in different ratios was used as mobile phase in gradient elution. ESI＋ and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 9 algal toxins were kept in definite ranges. Detection limits of the method ranged from 0.084 to 0.175 μg · L^-1. On the base of blank sample, test for recovery was made by standard addition methodl values of recovery found were in the range of 79.4%-113%, with RSDs （n=7） in the range of 5.1%-14%.