Dipartimento di Chimica, Università della Calabria, via P. Bucci cubo 12/C I-87030 Arcavacata di Rende (CS), Italy.
Rapid Commun Mass Spectrom. 2009 Dec;23(23):3803-6. doi: 10.1002/rcm.4324.
A new approach for the assay of rotenone (1) by isotope dilution mass spectrometry is presented. The extreme toxicity of rotenone, a natural phytodrug with insecticidal and piscicidal activity, recently banned by national and international environmental protection agencies, calls for the development of sensitive and accurate methods of analyses. Accordingly, the proposed protocol is based on the availability of the labeled internal standard rotenone-d3 (3) which can be conveniently prepared by consecutive and specific mono-O-demethylation, and remethylation with methyl iodide-d3. The sensitivity of the method is confirmed by the very low limit of detection (LOD) and quantitation (LOQ) values achieved in the assay of 1 in two distinct fortified matrices, and is further supported by the observed accuracy values.
本文提出了一种利用同位素稀释质谱法测定鱼藤酮（1）的新方法。鱼藤酮是一种天然植物药物，具有杀虫和杀鱼活性，毒性极强，最近已被国家和国际环境保护机构禁用，因此需要开发灵敏、准确的分析方法。因此，该方法基于标记内标鱼藤酮-d3（3）的可用性，该内标可通过连续且特异性的单-O-去甲基化和与碘甲烷-d3 的再次甲基化来方便地制备。该方法的灵敏度通过在两种不同强化基质中测定 1 时获得的非常低的检测限（LOD）和定量限（LOQ）值得到证实，并通过观察到的准确度值得到进一步支持。
