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目的建立测定贝类组织中腹泻性贝类毒素大田软海绵酸(okadaic acid,OA)的优化高效液相色谱-串联质谱方法。方法样品经0.125 mol/L盐酸性水溶液提取,乙酸乙酯萃取,HLB固相萃取小柱净化,采用液相色谱-串联质谱进行检测。结果以80%甲醇-水为流动相等度洗脱,流速为0.3 m L/min,柱温为35℃,选择正离子扫描和多反应监测(MRM)模式进行分析,OA在2~200μg/L范围内线性关系良好。采用本研究改进的前处理方法,4个添加水平下的回收率为90.5%~99.6%,高于采用行业标准SN/T2269-2009前处理方法的回收率(81.3%~87.5%),相对标准偏差小于10%,方法定量限(以S/N≥10计)为1.0μg/kg。成功应用本方法检测了湛江市市售的7种贝类样品,未检出OA。结论该优化方法灵敏度高,操作较简便,适合于多种贝类样品中OA的检测。
OBJECTIVE To establish a method for the determination of okadaic acid (OA) in diarrhea shellfish toxin in shellfish tissues by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with 0.125 mol / L hydrochloric acid aqueous solution, extracted with ethyl acetate, HLB solid phase extraction cartridges, and detected by liquid chromatography-tandem mass spectrometry. Results The mobile phase was eluted with 80% methanol-water as mobile phase at a flow rate of 0.3 m L / min and a column temperature of 35 ° C. Positive ion scan and MRM modes were used for the analysis. OA ranged from 2 to 200 μg / L Linear relationship within the range of good. Using the improved pretreatment method of this study, the recoveries at the four addition levels ranged from 90.5% to 99.6%, higher than those obtained using the industry standard SN / T2269-2009 pretreatment method (81.3% -87.5%), and the relative standard Deviations of less than 10%, the method of quantitative limits (S / N ≥ 10 meter) was 1.0μg / kg. This method was successfully applied to the detection of Zhanjiang City, seven kinds of shellfish samples were not detected OA. Conclusion The optimized method has high sensitivity, simple operation and is suitable for the detection of OA in many shellfish samples.