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样品毒素谱对用于官方麻痹性贝类毒素控制的高效液相色谱法适用性的影响。

Influence of the sample toxic profile on the suitability of a high performance liquid chromatography method for official paralytic shellfish toxins control.

作者信息

Ben-Gigirey B, Rodríguez-Velasco M L, Villar-González A, Botana L M

机构信息

Community Reference Laboratory of Marine Biotoxins (CRLMB), Agencia Española de Seguridad Alimentaria, Estación Marítima S/N, Muelle de Trasatlánticos, 36200 Vigo, Spain.

出版信息

J Chromatogr A. 2007 Jan 26;1140(1-2):78-87. doi: 10.1016/j.chroma.2006.11.048. Epub 2006 Nov 30.

Abstract

An HPLC-FLD method, involving pre-chromatographic oxidation of the PSP toxins with hydrogen peroxide and periodate, has been AOAC validated through a collaborative trial and adopted as AOAC Official Method. This method could be a candidate for replacing the mouse bioassay (MBA) for the Official Control of PSP toxins at European level, once accepted by the legislation. An interlaboratory exercise has been organized by the CRLMB to evaluate its "fitness for purpose" for the Official Control of PSP toxins in the EU laboratories. Eighteen EU laboratories took part in the study and had to analyze six bivalve mollusc samples with several PSP toxic profiles. The performance of the participant laboratories in the application of this method was compared with that obtained at the collaborative trial. Information on problems/drawbacks encountered by participants in the application of this method was also sought. The HPLC validated method is only applicable for Official PSP Control for certain samples. This depends on sample PSP toxic profile. Results obtained for samples where only GTX2,3 and STX were present were satisfactory and in agreement with MBA results. Results obtained for a sample with a toxic profile dominated by GTX6 and suspected to contain also C1,2 and C3,4 were not satisfactory. GTX5 and dc-STX could be quantified, although the results achieved (total toxicity) were lower than those obtained by MBA. It can be also useful as a screening method, complementary to MBA, helping in the reduction of the animals used. However, the lack of several PSP standards, the fact that the method is not validated for all the PSP toxins, and several drawbacks found in its application are a handicap to fully implement it for Official PSP Control as a viable replacement for bioassay.

摘要

一种高效液相色谱 - 荧光检测法(HPLC - FLD),该方法涉及用过氧化氢和高碘酸盐对麻痹性贝类毒素(PSP毒素)进行色谱前氧化,已通过协作试验获得AOAC验证,并被采纳为AOAC官方方法。一旦获得立法认可,该方法有望在欧洲层面替代小鼠生物测定法(MBA)用于PSP毒素的官方控制。欧洲海洋与淡水研究协调实验室(CRLMB)组织了一次实验室间比对活动,以评估该方法在欧盟实验室用于PSP毒素官方控制的“适用性”。18个欧盟实验室参与了此项研究,他们需要分析6个具有多种PSP毒素谱的双壳贝类软体动物样本。将参与实验室应用该方法的表现与协作试验中的结果进行了比较。同时还收集了参与者在应用该方法过程中遇到的问题/缺陷的相关信息。经过验证的HPLC方法仅适用于对某些样本进行PSP毒素的官方控制。这取决于样本的PSP毒素谱。对于仅含有GTX2、3和STX的样本,所得结果令人满意,且与小鼠生物测定法的结果一致。对于一个以GTX6为主且疑似还含有C1、2和C3、4的毒素谱样本,所得结果并不理想。GTX5和dc - STX可以进行定量分析,尽管所得结果(总毒性)低于小鼠生物测定法的结果。它也可作为一种筛查方法,作为小鼠生物测定法的补充,有助于减少实验动物的使用。然而,缺乏多种PSP标准品、该方法未针对所有PSP毒素进行验证以及在应用中发现的一些缺陷,阻碍了其作为生物测定法的可行替代方法全面用于PSP毒素的官方控制。

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