超高效液相色谱法快速测定贝类中的软骨藻酸残留
UHPLC Rapid Determination of Residual Domoic Acid in Shellfishes
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摘要: 利用超高效液相色谱快速测定贝类中的软骨藻酸残留。样品经甲醇(1+1)溶液提取,采用Oasis MAX固相萃取柱对提取液进行净化后,在Waters ACQUITY UPLC BEH C18色谱柱上分离,以乙腈-0.1%(体积分数)三氟乙酸(13+87)混合液为流动相进行洗脱,紫外检测波长为242 nm。软骨藻酸的线性范围为0.1~10.0 mg·L-1,测定下限(10S/N)为0.2 mg·kg-1。加标回收率在76.8%~91.2%之间,测定值的相对标准偏差(n=6)在11%~16%之间。Abstract: UHPLC was applied to the determination of residual domoic acid in shellfishes. The sample was extracted with methanol (1+1) solution. The extract was purified on Oasis MAX solid extraction column and the supernatant was separated on Waters ACQUITY UPLC BEH C18 chromatographic column with acetonitrile-0.1% (φ) trifluoroacetic acid solution (13+87) as the mobile phase for isocratic elution. UV-detection was made at the wavelength of 242 nm. The linearity range of domoic acid was 0.1-10.0 mg·L-1, with the lower limit of determination (10S/N) of 0.2 mg·kg-1. Recovery rates obtained by standard addition method were in the range of 76.8%-91.2%, and RSDs (n=6) were in the range of 11%-16%.