摘要
本文采用2-甲基-3-甲氧基-4-苯基丁酸(MMPB)衍生化法结合分散液液微萃取和气相色谱-质谱法发展了一种快速简便地检测水体中微囊藻毒素(MCs)总量的分析方法。考察了pH值、萃取剂的种类、萃取剂的用量和离心时间等参数的影响,并在优化条件下采用气相色谱-质谱法对水中的微囊藻毒素进行检测。分散液液微萃取(DLLME)条件为:在室温下,四氯乙烯体积为150μL、分散剂体积是0.5mL、超声时间为5min、离心10min。在0~10μg/L范围内MCs的浓度与对应的色谱峰面积呈现良好的线性关系,线性回归方程为y=1.01152×10^7+2.94041×10^8x(R^2=0.966),本方法对MCs的检出限为32.5ng/L,对MCs回收率均大于85.3%。
An analytical method for quick and easy determination of the total quantity of microcystins in water was developed by combining derivative MMPB with DLLMME and GC-MS.In this paper,the influencing parameters on the recovery of MMPB,such as initial pH,extraction solvent and its’dosages,centrifugal time,were investigated.The content of MCs in the water was studied by using gas chromatography-mass spectrometry in the optimized conditions.It is found that the conditions for DLLMME were:the extraction solvent of perchloroethylene was 150μL,0.5 ml methanol as the dispersant,ultrasonic time is 5 minutes,and centrifugalization for 10 minutes in 4000r/min with room temperature.There was a good linear relationship between the concentration of MCs and the corresponding chromatographic peak area in the range of 0~10 ug/L,and the linear regression equation was y=1.01152×10^7+2.94041×10^8x(R^2=0.966),and the detection limit with this method is 32.5ng/L,and the recovery rates are above 85.3%.
作者
宋兴良
冯晓阳
李娜
SONG Xing-liang;FENG Xiao-yang;LI Na(School of Chemistry&Chemical Engineering,Linyi University,Linyi Shandong 276005,China)
出处
《临沂大学学报》
2019年第6期1-8,共8页
Journal of Linyi University
基金
国家自然科学基金资助项目（21275068）
山东省自然科学基金（ZR2016BL25）资助
关键词
微囊藻毒素
2-甲基-3-甲氧基-4-苯基丁酸
分散液液微萃取
气相色谱-质谱法
microcystins(MCs)
2-methyl-3-methoxy-4-phenylbutyric acid(MMPB)
dispersive liquid-liquid microextraction(DLLMME)
gas chromatography-mass spectrometry(GC-MS)
