高效液相色谱串联质谱法测定水体中氨基脲、5-甲基吗啉-3-氨基-2-恶唑烷基酮、1-氨基乙内酰脲和3-氨基-2-唑烷基酮

Determination of semicarbazide,3-amino-5-morpholinomethy-1-2-oxazolidinone,1-aminohydation,3-amino-2-oxazolidinone in water by liquid chromatograghy-tandem mass spectrometry

建立了高效液相色谱三重四极杆串联质谱检测水体中痕量氨基脲(SEM)、5-甲基吗啉-3-氨基-2-恶唑烷基酮(AMOZ)、1-氨基乙内酰脲(AHD)和3-氨基-2-唑烷基酮(AOZ)的分析方法。水样在pH 1.5～3条件下衍生8 h,经乙酸乙酯萃取,氮吹浓缩,流动相溶解后,内标法定量。分析条件为:CAPCELLPAK C18色谱柱,以甲醇和2 mmol/L乙酸铵(含0.1%甲酸)溶液为流动相进行梯度洗脱。结果表明:AMOZ、AHD和AOZ在0.005～1μg/L范围内,SEM在0.01～1μg/L范围内呈现良好的线性关系,相关系数均大于0.9980。AMOZ、AHD和AOZ的定性检测限和定量检测限为分别为0.0025μg/L和0.005μg/L;SEM的定性检测限和定量检测限为分别为0.005μg/L和0.01μg/L。4种化合物在水体中3个不同浓度添加水平下的平均回收率为84.9%～110.4%,相对标准偏差为1.2%～7.8%。方法可用于分析环境水体中4种化合物的残留。

A fast, effective, and sensitive method for the simultaneous determination and confirmation of the trace levels of SEM, AMOZ, AOZ and AHD in water using Liquid chromatography-tandem mass spectrometry was developed. 500 mL of water samples were derivatized with nitrobenzaldehyde in pH 1.5 - 3 for 8 h, and extracted by ethyl acetate in slightalkali environment, and separated by a LC-column CAPCELL PAK Cls, then analyzed by clectrospray ionizations in positive mode with the selected reaction monitoring （SRM）. The results showed that the linear ranges were 0. 005 - 1μg/L for AHD,AMOZ,AOZ, and 0. 01 - 1μg/L for SEM, and the correlation coefficients were greater than 0. 9980. The determination limits of four compounds were 0. 0025μg/L （AHD,AMOZ,AOZ）, 0. 005μg/L（SEM）. The recoveries of four spiked at different concentration levels in blank samples were 84.9% - 110. 4% and the relative standard derivations （RSDs） of the method were in the range of 1.2% -7.8%.