摘要
建立强阳离子交换固相萃取一气相色谱/质谱(SCX/GC/MS)同时检测强离子干扰水中甲基膦酸(MPA)、异丙基膦酸(IPA)、甲基膦酸嚬哪酯(PMPA)、硫二甘醇(TDG)、硫二甘醇亚砜(TDGO)和硫二甘醇砜(TDGO2)的方法。利用优化的条件,测定TDGO在5.0～25 μ g/mL、其他化合物在2.5～25 μ g/mL的浓度范围内呈良好的线性关系,同时对浓度各为1.0μg/mL和10 μ g/mL的6种目标化合物的加标回收率均在34.1%～ 103.8%之间,且相对标准偏差均小于10%。该方法可实现强离子干扰水样中烷基膦酸的检测,有效避免真实样品中目标化合物的丢失,具有实用价值。
The strong cation exchange SPE for the methylphosphonic acid （MPA）, isopropylphosphonic acid （IPA）, pinacolyl methylphosphonic acid （PMPA）, and thiodiglycol （TDG）, thiodiglycol Sulfoxide （TDGO） and thiodiglycol Sulfone （TDGO2） in strong interferential aqueous liquid samples were systematically studied. Under the optimal conditions, the calibration curves showed good linearity in the range of 5.0-25μg/L for TDGO and 2.5-25 μg/L for rest of compounds. The LODs of all target compounds were 1.0 mg/L, and the recoveries of MPA, IPA, PMPA, TDG,TDGO and TDGO2 spiked at 1.0μg/L and 10.0μg/L ranged from 34.1%-103.8%, and the RSDs were less than 10% .Using the results, a large amount of inorganic cations is removed by strong cation exchanger （SCX）, and the new method improves the silylation efficiency of TDG, TDGO and TDGO2, and detection of alkylphosphonic acids in the strong ion interfering samples becomes possible.
出处
《现代仪器》
2009年第5期89-92,共4页
Modern Instruments
