Kataoka M, Tsuge K, Takesako H, Hamazaki T, Seto Y
National Research Institute of Police Science, 6-3-1 Kashiwanoha, Kashiwa, Chiba 277-0882, Japan.
Environ Sci Technol. 2001 May 1;35(9):1823-9. doi: 10.1021/es001529z.
Detection and identification of alkyl methylphosphonate (RMPA) and methylphosphonate (MPA) are performed to verify the existence of nerve gases by gas chromatography-mass spectrometry (GC-MS) after tert-butyldimethylsilylation (TBDMS). However, it is sometimes difficult to detect RMPA and MPA in soils. This study examines the relationship between the pedological characteristics and the aqueous extraction recoveries and TBDMS derivatization yields of ethyl-, isopropyl- and pinacolyl methylphosphonate and MPA for 21 soil samples. The aqueous extraction recoveries were measured directly by capillary electrophoresis. Andosols showed low extraction recoveries, while Regosols and Fluvisols showed high recoveries. RMPA were extracted with higher recoveries than MPA from all soils. MPA could not be extracted from Andosols. Within the pedological characteristics, phosphate absorption coefficients showed a strong negative correlation with the extraction recoveries of all phosphonates. The levels of RMPA and MPA in aqueous soil extracts were also determined for eight soils by GC-MS after TBDMS. Compared to the aqueous extraction recoveries, the yields of TBDMS derivatives were low. Strong anion exchange led to a significant improvement in derivatization yields. The efficiencies of TBDMS derivatization were inversely correlated with the levels of alkaline earth metals extractable from soils when the three soils that possessed high total carbon were excluded.
通过气相色谱 - 质谱联用仪(GC - MS)在叔丁基二甲基硅烷化(TBDMS)后对烷基甲基膦酸酯(RMPA)和甲基膦酸酯(MPA)进行检测和鉴定,以验证神经毒剂的存在。然而,有时在土壤中很难检测到RMPA和MPA。本研究考察了21个土壤样品的土壤学特征与乙基、异丙基和频哪基甲基膦酸酯以及MPA的水萃取回收率和TBDMS衍生化产率之间的关系。水萃取回收率通过毛细管电泳直接测定。火山灰土壤显示出较低的萃取回收率,而粗骨土和潮土显示出较高的回收率。在所有土壤中,RMPA的萃取回收率高于MPA。无法从火山灰土壤中萃取出MPA。在土壤学特征中,磷吸附系数与所有膦酸酯的萃取回收率呈强烈负相关。在TBDMS后,还通过GC - MS对8种土壤的水相土壤提取物中的RMPA和MPA水平进行了测定。与水萃取回收率相比,TBDMS衍生物的产率较低。强阴离子交换导致衍生化产率显著提高。当排除三种总碳含量高的土壤时,TBDMS衍生化效率与从土壤中可提取的碱土金属水平呈负相关。