摘要
采用无需衍生化的固相萃取为前处理手段,高效液相色谱-串联四极杆质谱联用技术(LCMSMS)为检测手段,在电喷雾电离正离子模式下,对澳大利亚畜牧业污水中常见的大环内酯和拟除虫菊酯两类共7种驱虫剂物质的残留,建立了一次进样下的有效快速分析方法。经一系列优化试验,确定了以50%丙酮+50%乙腈为洗提剂、每次4 mL共8 mL的洗提方法。结果表明,该固相萃取技术(SPE)的加标回收试验结果较好,各化合物的平均回收率为95.50%～108.00%,相对标准差范围为0.73%～8.82%。以含10 mmol/L醋酸铵、0.1%甲酸的超纯水和甲醇混合溶液为流动相,以准分子离子峰[M+NH4]^+、[M+H]^+作为母离子的定量离子对,所建立的1～500 ng/mL范围内的8点校正曲线中,各物质的相关系数均高于0.998 0,定量限范围为0.03～2.47 ng/mL。实际样品测定时,不同处理流程中各化合物的残留浓度有较好地体现。
The paper is aimed to introduce a method developed by the present authors for determining the concentration of seven kinds of parasiticides present in the feedlot sewage. For this purpose, we have adopted the integrated technology of high-performance liquid chro- matography and the tandem mass spectrometry （HPLC-MSMS）. Therefore, when we use the electric spray ionization （ESI） source and the positive ion model, the parameters of chromatography and spectrometry should be optimized..That is to say, when taking the solid phase extraction （SPE） as a pro-treating process, we should adopt the effluent half made of acetone and half made of acetonitrile, each time with the volume of 4mL of eluting and twice as much of eluting for the whole experiment. As a result, the recoveries of all the compounds from the spiking tests indicate that the method helps to enrich the seven target compounds with an average recovery ratio between 95.50% to 108.00%. Moreover, the methodological stability proves to be acceptable with the relative standard deviations （RSD） between 0.73% to 8.82%. Whereas mobile phase A proves to comprise ultra-pure water with 10 mmol/L ammonium acetate and 0.1% formic acid, mobile phase B should comprise 100% of methanol, with quasi-molecular ion peak [M ＋ NH4]^＋ and [M ＋ H]^＋ taking place in the full scan of the first quadrupole of the mass spectrometer （ QI ）. After the optimization, the two most intense precursor/product ion transitions should be selected for monitoring the corresponding analyte. And, finally, in determining the real sample from feedlot sewage, the method developed by the authors here represents a perfect profile to all the target compounds at different concentrations in each stage of treating process
出处
《安全与环境学报》
CAS
CSCD
北大核心
2009年第6期94-100,共7页
Journal of Safety and Environment
基金
澳大利亚肉类畜禽协会资助项目(FLOT.333)
作者简介
王松，工程师，从事水体及底泥中有机污染监测和防治研究，ws0506@163．com。
