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首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >Develop of a multiway chemometric-based analytical method fulfilling regulatory identification criteria: Application to GC-MS pesticide residue analysis
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Develop of a multiway chemometric-based analytical method fulfilling regulatory identification criteria: Application to GC-MS pesticide residue analysis

机译：满足法规鉴定标准的基于化学计量学的多方分析方法的开发：在GC-MS农药残留分析中的应用

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The proposed procedure is described by applying it to develop an analytical method which fulfils the SANCO specifications. Nevertheless, the procedure would be valid for any other legal specification that requires the identification of the analyte by means its m/. z values and retention time. To demonstrate the procedure, three herbicides (simazine, Sz; atrazine, Az; propazine, Pz), with terbuthylazine, Tz, as internal standard (IS) have been analysed by gas chromatography with mass spectrometry detection (GC/MS). The procedure consists of the following steps: (i) To record the data in the full scan mode (201 m/. z ratios). (ii) To select four characteristic ions which make possible the unequivocal identification of each triazine according to the criteria established in the Document SANCO/12495/2011 by means of principal components and hierarchical clustering of variables; (iii) To build a calibration based on the PARAFAC decomposition with the data recorded in SIM mode at the four m/. z ratios selected for each triazine. Afterwards several figures of merit have been evaluated. Bearing in mind that triazines are one of the most frequently used group of herbicides in agriculture and atrazine and simazine are included in the list of priority substances in Annex II of Directive 2008/105/EC, in this work, these analytes have been analysed in three natural waters. Prior to determination by gas chromatography with mass spectrometry detection (GC/MS) a step with solid phase extraction (SPE) has been carried out. The calibration set is made up of 40 standards 33 are external standards prepared in acetone and seven matrix matched prepared in deionised water subjected to the SPE procedure. Moreover, each kind of water, stream, well, and river, is analysed both unspiked and spiked. For the triazine determination, the second order PARAFAC advantage allows the use of samples prepared in acetone together with those prepared in deionised water subjected to SPE. The decision limit, CCα, and the capability of detection, CCβ, are calculated according to ISO 11843-2, assessing the false positive and false negative. The m/. z ratios chosen fulfils the SANCO identification criteria and also the spectrum obtained in the PARAFAC decomposition, which is common in all samples for each triazine. However, when the same experimental data are used to carry out a univariate calibration with the abundance of the base peak of each triazines, a lot of samples lie outside the permitted tolerances depending on the reference experimental spectra used, despite the fact that all of them have a triazine content above the detection limit. Also, the PARAFAC calibration allows us to detect the test samples which are not similar to the calibration samples and in this way their mistaken quantification is avoided.
机译：通过将其应用于开发满足SANCO规范的分析方法来描述所建议的过程。然而，该程序对于任何其他要求通过m /来鉴定分析物的法律规范都是有效的。 z值和保留时间。为了证明该方法，已通过气相色谱-质谱检测（GC / MS）分析了三种除草剂（西玛西嗪，Sz;阿特拉津，Az;丙嗪，Pz），其中叔丁嗪，Tz作为内标（IS）。该过程包括以下步骤：（i）以全扫描模式（201 m / .z比率）记录数据。 （ii）根据主要成分和变量的层次聚类，根据文件SANCO / 12495/2011中确立的标准，选择四个能够使每个三嗪明确鉴定的特征离子; （iii）基于PARAFAC分解，以SIM模式下以4 m /记录的数据建立校准。为每个三嗪选择z比。之后，已评估了几个优点。考虑到三嗪是农业中最常用的除草剂之一，而阿特拉津和西玛津被列入指令2008/105 / EC附件II的优先物质清单中，在这项工作中，对这些分析物进行了分析。三种天然水。在通过具有质谱检测（GC / MS）的气相色谱法进行测定之前，已经进行了具有固相萃取（SPE）的步骤。校准套件由40个标准品组成，其中33种是在丙酮中制备的外标，另外7种是在经过SPE程序的去离子水中配制成的基质。而且，对每种水，溪流，水井和河流都进行了非加标和加标分析。对于三嗪的测定，二阶PARAFAC的优势是可以使用在丙酮中制备的样品以及在经过SPE的去离子水中制备的样品。根据ISO 11843-2计算决策极限CCα和检测能力CCβ，评估假阳性和假阴性。 m /。所选的z比值既符合SANCO鉴定标准，也符合PARAFAC分解中获得的光谱，这在每种三嗪的所有样品中都是常见的。但是，当使用相同的实验数据对每种三嗪的基峰丰度进行单变量校正时，取决于所用的参考实验光谱，尽管有很多样品，但仍有许多样品超出了允许的公差范围。三嗪含量高于检测极限。同样，PARAFAC校准允许我们检测与校准样品不相似的测试样品，从而避免了错误的定量。

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