Li Shiyan, Wang Yang, Wang Dingnan, Wu Hongxi, Ding Xueyan, Cui Yiwei, Shen Qing
Aquatic Products Quality Inspection Center of Zhejiang Province, Hangzhou 310023, China.
Institute of Seafood, Zhejiang Gongshang University, Hangzhou 310012, China.
Se Pu. 2017 Aug 8;35(8):794-800. doi: 10.3724/SP.J.1123.2017.04018.
An analytical method was developed for the simultaneous and rapid determination of seven microcystins in fish meat by liquid chromatography-tandem mass spectrometry (LC-MS/MS) coupled with pass-through solid phase extraction (SPE). The samples were extracted with methanol-water (90:10, v/v) after heat treatment by water bath at 80℃, and then cleaned up with an Oasis PRiME HLB pass-through SPE column. The samples were analyzed directly on a Waters XSelect HSS T3 column using 0.1% (v/v) aqueous formic acid and acidified acetonitrile (0.1% formic acid, v/v) as mobile phases. Qualitative and quantitative analysis of the analytes was carried out under the multiple reaction monitoring mode with positive electrospray ionization. The matrix matching external standard method was used for quantitation analysis. To solve the problem of parent ion selection of the microcystins, the ionization characteristics of microcystins were evaluated under different mobile phase conditions. Finally, the results showed that the acid could promote the intensity of the doubly charged ions significantly. The calibration curves were linear well in the corresponding concentration ranges, with correlation coefficient ≥ 0.99. The limits of quantification ranged from 0.30 to 2.0 μ g/kg. The average spiked recoveries for the seven microcystins were between 70.6% and 96.1% with the relative standard deviations of 3.4%-9.6%. The proposed method is sensitive, accurate, and efficient. It is applicable for the determination of microcystins in fish meat.
建立了一种液相色谱 - 串联质谱（LC-MS/MS）结合在线固相萃取（SPE）同时快速测定鱼肉中七种微囊藻毒素的分析方法。样品经80℃水浴热处理后，用甲醇 - 水（90:10，v/v）提取，然后通过Oasis PRiME HLB在线SPE柱净化。样品直接在Waters XSelect HSS T3柱上进行分析，以0.1%（v/v）甲酸水溶液和酸化乙腈（0.1%甲酸，v/v）作为流动相。在正电喷雾电离的多反应监测模式下对分析物进行定性和定量分析。采用基质匹配外标法进行定量分析。为解决微囊藻毒素母离子选择问题，评估了不同流动相条件下微囊藻毒素的电离特性。结果表明，酸可显著提高双电荷离子强度。校准曲线在相应浓度范围内线性良好，相关系数≥0.99。定量限为0.30～2.0μg/kg。七种微囊藻毒素的平均加标回收率在70.6%～96.1%之间，相对标准偏差为3.4%～9.6%。该方法灵敏、准确、高效，适用于鱼肉中微囊藻毒素的测定。
