Lee Jin Young, Shin Ji Young, Kim Hyun Suk
ChemBio Technology Center, Agency for Defense Development, PO Box 35-5, Yuseong-gu, Daejeon 34186, Republic of Korea.
J Anal Toxicol. 2023 Feb 21;47(1):81-88. doi: 10.1093/jat/bkac028.
There have been no detailed investigations regarding solid-phase-extraction (SPE) optimization and screening for the degradation products of ethyl (1-(diethylamino)ethylidene)phosphoramidofluoridate (A234) in various environmental samples. Therefore, as a first step in the selective SPE of the degradation products of A234, we optimized the SPE adsorption and extraction parameters for the A234 degradation product ethylhydrogen (1-(diethylamino)ethylidene)phosphoramidate (cpd 1). Among various SPE cartridges, the Si cartridge (500 mg, 3 mL) selectively extracted cpd 1 using an elution volume of 4 mL of 25% H2O in acetonitrile, which eliminated most interference without cpd 1 loss during loading and washing. In addition, the sorbent capacity is also critical in the adsorption of cpd 1. The Si cartridge (500 mg, 3 mL) retained cpd 1 in the concentration range 1-10 µg/mL. The linearity of detector response of cpd 1 in deionized H2O was studied in the range of 1.0-100 ng/mL and showed good linearity with γ2 ranging from 0.9979 to 0.996. The limits of detection for cpd 1 are 10 ng/mL in the product-scan mode and 100 ng/mL in the full-scan mode. Also, after we optimized the SPE method, we validated the precision and accuracy of the Si-cartridge extraction method in real soil samples with diverse concentrations. The precision ranged from 2.5% to 5.3%. This newly developed SPE is applicable to the analysis of a degradation product of Novichok A234 in various environmental matrices, such as water, soil and sand, in the Organization for the Prohibition of Chemical Weapons (OPCW) proficiency test and unknown samples collected from suspected sites.
关于在各种环境样品中对乙基（1 - （二乙氨基）亚乙基）磷酰胺氟化物（A234）降解产物进行固相萃取（SPE）优化和筛选的详细研究尚未开展。因此，作为对A234降解产物进行选择性SPE的第一步，我们优化了A234降解产物乙基氢（1 - （二乙氨基）亚乙基）磷酰胺（化合物1）的SPE吸附和萃取参数。在各种SPE柱中，硅胶柱（500mg，3mL）使用4mL 25%水的乙腈洗脱液选择性地萃取化合物1，在加载和洗涤过程中消除了大部分干扰且化合物1无损失。此外，吸附剂容量对化合物1的吸附也至关重要。硅胶柱（500mg，3mL）在1 - 10μg/mL浓度范围内保留化合物1。在去离子水中研究了化合物1在1.0 - 100ng/mL范围内的检测器响应线性，γ2在0.9979至0.996范围内显示出良好的线性。化合物1在产物扫描模式下的检测限为10ng/mL，在全扫描模式下为100ng/mL。而且，在我们优化了SPE方法后，我们在不同浓度的实际土壤样品中验证了硅胶柱萃取方法的精密度和准确度。精密度范围为2.5%至5.3%。这种新开发的SPE适用于在禁止化学武器组织（OPCW）能力验证测试以及从疑似地点采集的未知样品中，对各种环境基质（如水、土壤和沙子）中的诺维乔克A234降解产物进行分析。
