Plant Protection Institute-National Research Institute, Regional Experimental Station, Laboratory of Pesticide Residues, Chelmonskiego 22, 15-195, Bialystok, Poland,
J Nat Med. 2014 Jan;68(1):95-111. doi: 10.1007/s11418-013-0777-9. Epub 2013 May 14.
In this study two analytical methods, one based on matrix solid phase dispersion (MSPD) and the other on liquid-solid extraction (LSE), coupled with gas chromatography, were evaluated and used to determine the presence of 163 pesticides (6 acaricides, 62 fungicides, 18 herbicides and 77 insecticides) in various herbs. Both methods were optimized considering different parameters (sample to sorbent mass ratio, extracting solvent, sorbents for clean-up step, etc.). The results of these validated sample preparation procedures were compared. Under optimum conditions, the mean recoveries obtained were in the range of 70-119% for MSPD for most pesticides and 70-118% for LSE, but with several exceptions. Precision values, expressed as relative standard deviation (RSD), were ≤16% for MSPD and <18% for LSE. Correlation coefficients were higher than 0.99254 for both methods. LODs (limits of detection) and LOQs (limits of quantification) for MSPD were within the ranges of 0.003-0.03 and 0.005-0.04 mg/kg, respectively. The data demonstrate that the MSPD method was successfully used for the analysis of 163 pesticides in the following herbs: chamomile (Matricaria chamomilla L.), linden (Tilia), lungwort (Pulmonaria L.), melissa (Melissa L.), peppermint (Mentha piperita L.) and thyme (Thymus vulgaris L.). This paper indicates the potential of MSPD for qualitative and quantitative analysis of pesticide residues. This method was therefore validated at three spiking levels (the first ranging from 0.005 to 0.05 mg/kg, the second from 0.05 to 0.5 mg/kg and the third from 0.25 to 2.5 mg/kg) and applied to real samples (n = 15). MSPD proves to be a simple, fast and very useful multiresidue method and can be recommended for routine pesticide monitoring studies in various herbs.
在这项研究中,评估并使用了两种基于基质固相分散(MSPD)和液-固萃取(LSE)的分析方法,将其与气相色谱法相结合,以确定各种草药中存在的 163 种农药(6 种杀螨剂、62 种杀菌剂、18 种除草剂和 77 种杀虫剂)。两种方法都考虑了不同的参数(样品与吸附剂的质量比、提取溶剂、净化步骤的吸附剂等)进行了优化。比较了这些经过验证的样品制备程序的结果。在最佳条件下,MSPD 对大多数农药的平均回收率范围为 70-119%,LSE 的回收率范围为 70-118%,但也有几个例外。MSPD 的精密度值(表示为相对标准偏差(RSD))为≤16%,LSE 的精密度值<18%。两种方法的相关系数均高于 0.99254。MSPD 的检出限(LOD)和定量限(LOQ)分别为 0.003-0.03 和 0.005-0.04mg/kg。数据表明,MSPD 方法成功地用于分析以下草药中的 163 种农药:洋甘菊(Matricaria chamomilla L.)、椴树(Tilia)、肺草(Pulmonaria L.)、香蜂草(Melissa L.)、薄荷(Mentha piperita L.)和百里香(Thymus vulgaris L.)。本文表明 MSPD 具有用于农药残留定性和定量分析的潜力。因此,该方法在三个加标水平(第一个水平范围为 0.005 至 0.05mg/kg,第二个水平范围为 0.05 至 0.5mg/kg,第三个水平范围为 0.25 至 2.5mg/kg)进行了验证,并应用于实际样品(n=15)。MSPD 证明是一种简单、快速且非常有用的多残留方法,可推荐用于各种草药中的常规农药监测研究。