Division of Agricultural Chemicals, ICAR-Indian Agricultural Research Institute, New Delhi, 110012, India; Division of Natural Resources Management, ICAR-Central Islands Agricultural Research Institute, Port Blair, 744105, India.
Division of Agricultural Chemicals, ICAR-Indian Agricultural Research Institute, New Delhi, 110012, India.
J Chromatogr A. 2024 Aug 16;1729:465012. doi: 10.1016/j.chroma.2024.465012. Epub 2024 May 17.
Acrylamide and N, N-methylene bis acrylamide are most commonly used monomer and crosslinker compounds employed in synthesis of super absorbent hydrogels. When applied as soil conditioners, there are apprehensions that these hydrogels degrade over time and thus may release the toxic monomers in the soil. A method was thus developed using Liquid Chromatography tandem mass spectrometry (LC-MS/MS) for the trace level quantification of acrylamide (AD), acrylic acid (AA) and N,N-methylene-bis-acrylamide (MBA) in sandy loam soil amended by two test hydrogels the Pusa Hydrogel and SPG 1118 hydrogel prepared using AD and MBA. The MRM (multiple reaction monitoring) transitions were optimized for both the compounds. Soil samples were extracted using dispersive solid-phase extraction (dSPE) with a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) technique, employing acetonitrile. All analytes were quantified at trace levels within a five-minute run using UHPLC equipped with a C-18 column. Single laboratory validation of the developed method in soil matrix was conducted based on specificity, linearity, sensitivity, accuracy, precision, matrix effect and measurement of uncertainty. LC-MS/MS exhibited a linear response in the concentration range of 0.001 to 1 µg mL, with correlation coefficient >+0.99. Acceptable recovery (within 70-120 %) with repeatability (%RSD ≤20 %) was obtained at 0.01 to 1 µg g fortification levels. LOQ (Limit of quantification) of the method for AD, AA and MBA in soil matrix were 0.05, 1 and 0.01 µg g, respectively. Both intra-laboratory repeatability and intermediate precision at LOQ suggested well acceptable precise (HorRat≈ 0.3) method for quantification. Matrix enhancement effect was observed in the order: AA>AD>MBA. The Expanded Uncertainty (EU) in soil matrix at LOQ was 21.64 %, 28 % and 19 % for AD, AA and MBA respectively. Groundnut and wheat grown with application of the hydrogels showed no detectable residues of monomers in soil samples (total n = 60) near the root zone at the time of crop harvesting.
丙烯酰胺和 N, N-亚甲基双丙烯酰胺是合成高吸水性水凝胶最常用的单体和交联剂化合物。当用作土壤改良剂时，人们担心这些水凝胶会随着时间的推移而降解，因此可能会将有毒单体释放到土壤中。因此，开发了一种使用液相色谱串联质谱（LC-MS/MS）的方法，用于痕量定量分析沙壤土中两种测试水凝胶（Pusa 水凝胶和使用 AD 和 MBA 制备的 SPG 1118 水凝胶）添加后的丙烯酰胺（AD）、丙烯酸（AA）和 N, N-亚甲基双丙烯酰胺（MBA）。对两种化合物的 MRM（多重反应监测）跃迁进行了优化。使用改良的 QuEChERS（快速、简单、廉价、有效、坚固、安全）技术，用乙腈从土壤样品中进行分散固相萃取（dSPE）提取。所有分析物都在配备 C-18 柱的 UHPLC 上，在五分钟的运行时间内以痕量水平定量。在土壤基质中对开发方法进行了单实验室验证，包括特异性、线性、灵敏度、准确性、精密度、基质效应和不确定度测量。LC-MS/MS 在 0.001 至 1 µg mL 的浓度范围内表现出线性响应，相关系数>+0.99。在 0.01 至 1 µg g 的添加水平下，可获得可接受的回收率（70-120%）和重复性（%RSD ≤20%）。AD、AA 和 MBA 在土壤基质中的方法 LOQ（定量下限）分别为 0.05、1 和 0.01 µg g。LOQ 时的实验室内重复性和中间精密度表明，该方法的定量结果具有很好的可接受精度（HorRat≈0.3）。观察到基质增强效应的顺序为：AA>AD>MBA。在 LOQ 时，AD、AA 和 MBA 在土壤基质中的扩展不确定度（EU）分别为 21.64%、28%和 19%。在作物收获时，靠近根区的土壤样品（总 n=60）中未检测到水凝胶应用后单体的残留。
