一种简便的高效液相色谱法，用于检测以9-蒽甲酯形式存在的冈田酸类似物，并通过柱切换实现自动样品净化。

A convenient HPLC method for detection of okadaic acid analogs as 9-anthrylmethyl esters with automated sample cleanup by column switching.

作者信息

Uchida Hajime, Watanabe Ryuichi, Matsushima Ryoji, Uchida Naoyuki, Nagai Hiroshi, Kamio Michiya, Murata Masakazu, Yasumoto Takeshi, Suzuki Toshiyuki

出版信息

J AOAC Int. 2014 Mar-Apr;97(2):391-7. doi: 10.5740/jaoacint.sgeuchida.

DOI:10.5740/jaoacint.sgeuchida

PMID:24830150

Abstract

A convenient HPLC-fluorometric detection (FLD) method for okadaic acid (OA) analogs as 9-anthrylmethyl esters was developed with the addition of column switching to simplify and automate cleanup. Methanol extracts of shellfish were first treated to hydrolyze OA esters and then reacted with 9-anthryldiazomethane (ADAM). ADAM derivatives of OA and dinophysistoxin-1 (DTX1) were subsequently determined by HPLC-FLD following automated column-switching cleanup. The LOD (S/N = 3) and LOQ (S/N = 10) of OA and DTX1 obtained from bivalves fortified with toxin in our method were approximately 2.6 and 8.6 ng/g whole meat, respectively. The recoveries of OA and DTX1 at all fortification levels of bivalve extracts ranged from 90 to 113%, with RSD values of 0.9-9.9%. The new method is applicable to the routine monitoring of OA analogs as an inexpensive and convenient alternative to HPLC/MS.

摘要

开发了一种便捷的高效液相色谱 - 荧光检测（FLD）方法，用于检测作为9 - 蒽甲基酯的冈田酸（OA）类似物，并增加了柱切换功能以简化和自动化净化过程。贝类的甲醇提取物首先经过处理以水解OA酯，然后与9 - 蒽重氮甲烷（ADAM）反应。随后，通过自动柱切换净化后的高效液相色谱 - 荧光检测法测定OA和鳍藻毒素 - 1（DTX1）的ADAM衍生物。在我们的方法中，从添加毒素的双壳贝类中获得的OA和DTX1的检测限（S/N = 3）和定量限（S/N = 10）分别约为2.6和8.6 ng/g全肉。双壳贝类提取物在所有强化水平下OA和DTX1的回收率为90%至113%，相对标准偏差值为0.9 - 9.9%。该新方法适用于OA类似物的常规监测，是一种比高效液相色谱/质谱法更便宜、更便捷的替代方法。