分散固相萃取法测定黄瓜中的喹啉铜残留量
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摘要
建立了分散固相萃取(d-SPE)-高效液相色谱(HPLC)分析测定黄瓜中喹啉铜残留量的方法。样品采用乙腈和0.1 mol/L盐酸混合溶液提取,C18填料净化,高效液相色谱仪分离,紫外检测器检测。其色谱条件为:色谱柱SunFireC18(4.6×150 mm,5μm),流动相为十二烷基硫酸钠磷酸盐缓冲液-乙腈(65∶35)体系,流速0.6 mL/min,检测波长250nm。结果表明:在0.02、0.2、2 mg/kg三个添加水平下,喹啉铜回收率在92.3%～107.7%之间,相对标准偏差(RSD)在2.0%～7.7%之间。该方法操作简单、灵敏度和准确度高,能够用于黄瓜中喹啉铜的残留分析。
A high performance liquid chromatography(HPLC) coupled with the dispersive solid phase extraction(d-SPE) method for the determination of oxine-copper residue in cucumber was established. The sample was extracted by acetonitrile and hydrochloric acid(0.1 mol/L). The extract was purified by C_(18). The analysis was carried out by phosphate buffer saline(PBS) and sodium dodecyl sulfate(SDS)-acetonitrile(65:35) at a flow rate of 0.6 mL/min on SunFireC_(18)(4.6×150 mm, 5 μm) column, and detected by HPLC with UV detector at a ultraviolet absorption wavelength of 250 nm. The recovery was in 92.3%-107.7% with relative standard deviation(RSD) of 2.0%-7.7% at spiked levels of 0.02, 0.2 and 2 mg/kg. The method is simple, sensitive and accurate, and could be used in the determination of oxine-copper residue in cucumber.
A high performance liquid chromatography(HPLC) coupled with the dispersive solid phase extraction(d-SPE) method for the determination of oxine-copper residue in cucumber was established. The sample was extracted by acetonitrile and hydrochloric acid(0.1 mol/L). The extract was purified by C_(18). The analysis was carried out by phosphate buffer saline(PBS) and sodium dodecyl sulfate(SDS)-acetonitrile(65:35) at a flow rate of 0.6 mL/min on SunFireC_(18)(4.6×150 mm, 5 μm) column, and detected by HPLC with UV detector at a ultraviolet absorption wavelength of 250 nm. The recovery was in 92.3%-107.7% with relative standard deviation(RSD) of 2.0%-7.7% at spiked levels of 0.02, 0.2 and 2 mg/kg. The method is simple, sensitive and accurate, and could be used in the determination of oxine-copper residue in cucumber.
引文
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[14]周梦春,周华伦,阿加尔古丽·赛依提.番茄中8-羟基喹啉铜残留量的液相色谱测定[J].干旱环境监测,2010,24(4):205-208.
[15]丁明玉,王宗花,郑睿.多壁碳纳米管固相萃取填料对芳香化合物的吸附机理研究[J].分析试验室,2010,29(1):18-20.
[2]陈娇领,陈军辉.喹啉铜的合成工艺设计[J].煤炭与化工,2013,36(6):88-90.
[3]Theophanides T,Anastassopoulou J.Copper and carcinogenesis[J].Critical Reviews in Oncology/Hematology,2002,42(1):57-64.
[4]Listed N.Some fumigants,the herbicides 2,4-D and 2,4,5-T,chlorinated dibenzodioxins and miscellaneous industrial chemicals[J].IARC Monographs on the Evaluation of the Carcinogenic Risk of Chemicals to Man 1977,15:1-354.
[5]王志新,姚杰,刘传德,等.苹果中喹啉铜残留的GC测定方法探讨[J].农学学报,2015,5(12):51-54.
[6]姚杰,刘传德,周先学,等.气相色谱-氮磷检测法检测喹啉铜在苹果中的残留及消解动态[J].农药学学报,2016,18(1):130-134.
[7]李雨晨,李腾,邓立刚,等.超高效液相色谱法测定西瓜中的喹啉铜残留量[J].分析测试学报,2014,33(8):951-954.
[8]张培志,吴军,刘继东,等.高效液相色谱法分离检测8-羟基喹啉和8-羟基喹啉铜[J].分析化学,2003(9):1150.
[9]范珺,王明林,于建垒,等.黄瓜中霜脲氰和喹啉铜的残留检测及膳食风险评估[J].山东农业科学,2014,46(5):122-126.
[10]周梦春,蔡磊明,王捷,等.反相离子对色谱法测定土壤中喹啉铜的残留量[J].农药,2008,47(10):754-756.
[11]李国平,单炜力,王国联.高效液相色谱法测定混剂中喹啉铜和噻菌灵[J].农药科学与管理,2005,26(9):4-6.
[12]肖浩,龚道新,吴亮,等.高效液相色谱法测定稻田样品中喹啉铜残留[J].农药学学报,2015,17(1):106-110.
[13]周梦春,舒耀皋,王颖,等.反相高效液相色谱法测定黄瓜和土壤中的喹啉铜残留量[J].新疆农业大学学报,2008,31(4):47-49.
[14]周梦春,周华伦,阿加尔古丽·赛依提.番茄中8-羟基喹啉铜残留量的液相色谱测定[J].干旱环境监测,2010,24(4):205-208.
[15]丁明玉,王宗花,郑睿.多壁碳纳米管固相萃取填料对芳香化合物的吸附机理研究[J].分析试验室,2010,29(1):18-20.