CAJ | 학술논문

建立了沉积物中痕量十溴联苯醚的分散液液微萃取-上浮溶剂固化-高效液相色谱-紫外法(DLLME-SFO-HPLC-UV).以正交试验数据为训练样本,采用BP(Baek propagation)神经网络模型优化了分散液液微萃取-上浮溶剂固化条件:分散剂为1.00 mL甲醇、萃取剂为35.μL十二醇、Nacl质量浓度为10.00%、萃取时间10 min和pH=5,其萃取率(ER)可达62.22%.方法的线性范围为3.5～1400 ng/g(r=0.9960),检出限(LOD)和定量限(LOQ)分别为2.3 pg/g(s/N=2)和5.6 pg/g(s/N=5),实际样品的加标回收率为97.7%～104.2%.本方法集萃取、富集、分离步骤于一体,简化了沉积物中十溴联苯醚的前处理过程.
건립료침적물중흔량십추련분미적분산액액미췌취-상부용제고화-고효액상색보-자외법(DLLME-SFO-HPLC-UV).이정교시험수거위훈련양본,채용BP(Baek propagation)신경망락모형우화료분산액액미췌취-상부용제고화조건:분산제위1.00 mL갑순、췌취제위35.μL십이순、Nacl질량농도위10.00%、췌취시간10 min화pH=5,기췌취솔(ER)가체62.22%.방법적선성범위위3.5～1400 ng/g(r=0.9960),검출한(LOD)화정량한(LOQ)분별위2.3 pg/g(s/N=2)화5.6 pg/g(s/N=5),실제양품적가표회수솔위97.7%～104.2%.본방법집췌취、부집、분리보취우일체,간화료침적물중십추련분미적전처리과정.
A method for the determination of decabrominated diphenyl ether(decaBDE) in sediment samples at trace level using dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) and high performance liquid chromatography-ultraviolet detector (HPLC-UV) has developed.Based on the data of interactive orthogonal array design, the optimization experimental conditions were obtained with BP artificial neural network model: 1.00 mL methanol as dispersive solvent, 35.0 μL dodecanol as extractive solvent, 10.00% NaCl, pH 5, and extraction in 10 min.The extraction recovery (ER) was 62.22% at the extraction conditions.The proposed method exhibited a wide linear range(3.5-1400 ng/g) with R~2 =0.9921.The limit of detection (LOD) and the limit of quantification (LOQ) of this method were 2.3 pg/g(S/N =2) and 5.6 pg/g(S/N = 5), respectively.The recoveries of real samples at different spiking levels of decaBDE were 104.2%, 98.4% and 97.7%, respectively.Extraction, concentration and separation procedures for decaBDE from the sediment sample were carried out by one step, and hence, the process of DLLME-SFO for decaBDE was shortened.