摘要
目的:建立简便、灵敏、准确的测定水中11种痕茸N-甲基氨基甲酸酯类农药及其代谢产物的固相萃取、高液相色谱柱后衍生的检测方法。方法:水样经ODS—C18小柱富集、净化后,以甲醇/TL/乙腈为流动相,在Waters氨基甲酸酯类农药分析专用柱(3.9mm×150mm)上进行梯度洗脱分离,然后再在碱性条件下(pH〉9.0),采用2-巯基乙醇和邻苯二甲醛(OPA)进行柱后衍生,荧光法检测(λex339nm,λem445nm)。结果:11种N-甲基氨基甲酸酯类农药及其代谢产物在50.0—1500.0μg/L范围内均具有良好的线性,水样的定量检测下限为0.10—0.73μg/L,方法回收率在91.5%~104.1%,RSD均小于7.6%。结论:该法灵敏度高、操作简便、快速,适用于实际样品的测定。
Objective:To establish a simple, sensitive and exact method for the determination of eleven trace N - methycarbamates in water by solid phase extraction and HPLC with post - column derivatization. Methods:The water samples were extracted and condensed by solid - phase extraction with ODS - C18 cartridges, and then were separated on a Carbamate Analysis HPLC column (3.9 mm×150 mm) using a gradient mobile phase consisting of CH3OH - CH3CN - H2O at a flow rate of 1.50 ml/min. Detection was performed on a fluorescence detector( λex 339 nm ,λem 445 nm) after post - column derivazation with O - phthalaldehyde (OPA) and 2 - Mercaptoethanol ( 2 - Me) in the sodium hydroxide solution ( pH 〉 9 ). Results : The linear range of the eleven N - methycarbamates was 50. 0 - 1 500.0μg/L and the detection limits for quantification were 0. 10-0. 73μg/L. Extraction recoveries were between 91.5%- 104. 1%, and RSD were less than 7.6%. Conclusion:This method is found to be sensitive, fast and simple. Therefore, it can be used for the determination of the eleven trace N - methycarbamates in water samples.
出处
《中国卫生检验杂志》
CAS
2006年第1期9-11,共3页
Chinese Journal of Health Laboratory Technology
基金
宁波市医学科研基金项目(NB2003056)