中文摘要：

将固相萃取（SPE）和高效液相色谱-串联质谱（LC-MS/MS）结合,建立了河水样品中5种有机磷酸酯（OPEs）代谢物的分析方法。样品过滤后,使用HLB固相萃取小柱进行富集净化,采用6 m L甲醇洗脱后氮吹定容。以Luna Phenyl-Hexyl色谱柱为分离柱,甲醇和50 mmol·L-1乙酸铵水溶液为流动相梯度洗脱,在电喷雾负离子模式下,采用多反应监测模式（MRM）进行测定。优化条件下,仪器测定限（IDL）为0.002~1.15μg·L~（-1）,方法检出限（MDL）为0.15~4.48 ng·L~（-1）,实际水样加标浓度为10 ng·L~（-1）和50 ng·L~（-1）时回收率分别为54.1%~83.6%和57.8%~102%,相对标准偏差（RSD）分别为5.3%~19.5%和2.8%~15.7%。考察了基质效应对5种化合物分析的影响,同时应用该方法对武汉7个湖水样品进行分析,除DEHP外其它4种OPEs代谢物均有检出。该方法具有良好的精密度和准确度,可用于有机磷酸酯代谢物的环境行为研究。

英文摘要：

A liquid chromatography- tandem mass spectrometric（ LC- MS / MS） method was developed for the determination of five organophosphate ester metabolites in river water samples. The filtered water samples were enriched and purified by solid phase extraction（ SPE） using a HLB cartridges,and then eluted with 6 m L methanol. The eluent was concentrated to a volume of 0. 5 m L under gentle nitrogen stream and then diluted to 1 m L by initial mobile phase（ 50% methanol）. Instrumental analysis was accomplished by HPLC- MS / MS under negative electrospray ion and multiple reaction monitoring（ MRM） mode. Separation of the analytes was performed on a Luna Phenyl- Hexyl column,and a mixture of methanol and 50 mmol · L~（-1）ammonium acetate solution was selected as mobile phase for gradient elution. The recoveries of five organophosphate ester metabolites in river samples were in the range of 57. 8%~（-1）02% at a spiked concentration of 50 ng·L~（-1）with relative standard deviations（ RSD） of 2. 8%~（-1）5. 7%. At a spiked concentration of 10 ng·L~（-1）,the recoveries were in the range of 54. 1%- 83. 6% with RSDs of 5. 3%~（-1）9. 5%. The instrumental detection limits（ IDL） ranged from 0. 002 μg · L~（-1）to 1. 15 μg · L~（-1）and the method detection limits（ MDL） ranged from 0. 15 ng·L~（-1）to 4. 48 ng·L~（-1）. The matrix effect of river samples was also in-vestigated in this study. The proposed method was successfully applied in the determination of organophosphate ester metabolites in lake water samples collected from Wuhan, Hubei. Except for DEHP,the other four OPEs metabolites were all detectable in lake water. The method showed good precision and accuracy,and was suitable for the analysis of five organophosphate ester metabolites in surface water samples.