Phosiri Preeyaporn, Pongpinyo Prachathipat, Santaladchaiyakit Yanawath, Burakham Rodjana
Materials Chemistry Research Center, Department of Chemistry, Faculty of Science, Khon Kaen University Khon Kaen 40002 Thailand
Agricultural Production Sciences Research and Development Office, Department of Agriculture Bangkok 10900 Thailand.
RSC Adv. 2023 Mar 16;13(13):8863-8872. doi: 10.1039/d2ra07704c. eCollection 2023 Mar 14.
A green solvent of ternary deep eutectic solvent (menthol-thymol-dodecanoic acid) was prepared and used as a functional reagent to modify a magnetic mixed iron hydroxide@MIL-101(Cr)-NH composite. The proposed sorbent (MIH@MIL-101(Cr)-NH-TDES) was applied in magnetic solid phase extraction (MSPE) for the enrichment of organochlorine pesticides. The analytes were quantitively analyzed by GC-MS. The relationships of experimental parameters for preparing the proposed sorbent and the MSPE method were studied through a Box-Behnken design and a central composite design, respectively. Their optimized conditions were investigated using response surface methodology. Application of the MIH@MIL-101(Cr)-NH-TDES sorbent in MSPE successfully enhanced the sensitivity of GC-MS analysis, giving enrichment factors in the range of 56-168. The MSPE/GC-MS method was developed using MIH@MIL-101(Cr)-NH-TDES as a sorbent and was successfully employed for the preconcentration/determination of organochlorine residues in honey and tea samples. The satisfactory detection limits were in the ranges of 0.07-0.80 ng g and 0.7-8.5 ng g for honey and tea samples, respectively. Acceptable recoveries were obtained in the ranges of 81.7-107.3% and 85.4-109.3% for the spiked honey and tea samples, respectively, with RSDs lower than 10.0%.
制备了一种三元深共熔溶剂（薄荷醇-百里酚-十二烷酸）绿色溶剂，并将其用作功能试剂来改性磁性混合氢氧化铁@MIL-101(Cr)-NH复合材料。所提出的吸附剂（MIH@MIL-101(Cr)-NH-TDES）应用于磁性固相萃取（MSPE）中以富集有机氯农药。通过气相色谱-质谱联用（GC-MS）对分析物进行定量分析。分别通过Box-Behnken设计和中心复合设计研究了制备所提出吸附剂的实验参数与MSPE方法之间的关系。使用响应面方法研究了它们的优化条件。MIH@MIL-101(Cr)-NH-TDES吸附剂在MSPE中的应用成功提高了GC-MS分析的灵敏度，富集因子在56-168范围内。以MIH@MIL-101(Cr)-NH-TDES作为吸附剂建立了MSPE/GC-MS方法，并成功用于蜂蜜和茶叶样品中有机氯残留的预浓缩/测定。蜂蜜和茶叶样品的满意检测限分别在0.07-0.80 ng/g和0.7-8.5 ng/g范围内。加标蜂蜜和茶叶样品的回收率分别在81.7-107.3%和85.4-109.3%范围内，相对标准偏差低于10.0%。
