QuEChERS-SPE结合超高效液相色谱-质谱/质谱仪测定动物肝脏中的万古霉素和去甲万古霉素残留量
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摘要
建立了QuEChERS-SPE结合超高效液相色谱-质谱/质谱仪(UPLC-MS/MS)测定动物肝脏中万古霉素和去甲万古霉素残留量的方法。肝脏样品采用0. 1%甲酸水-乙腈溶液进行提取,乙二胺-N-丙基硅烷(PSA)吸附剂和十八烷基硅烷键合硅胶(C_(18))吸附剂初步净化,再用Strata-X-C固相萃取柱进行净化,UPLC-MS/MS正离子模式扫描,多反应监测模式(MRM)测定,外标法定量。结果表明,QuEChERS-SPE双重净化可有效降低肝脏基质中杂质的干扰,万古霉素和去甲万古霉素在5. 0～100. 0μg/L浓度范围内线性关系良好(线性相关系数均大于0. 999),检出限为2. 0μg/kg,定量限为5. 0μg/kg,加标平均回收率在78. 6%～90. 3%。该方法灵敏度高,准确度好,能满足对动物肝脏中万古霉素和去甲万古霉素定量分析的要求。
To establish a method for the determination of vancomycin and norvancomycin residue in animal liver based on Qu EChERS-SPE by ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS). The samples were extracted with mixed solution of 0. 1% formic acid and acetonitrile,purified first by PSA and C_(18),then cleaned with solid phase extraction( Strata-X-C),determined by UPLC-MS/MS with positive electrospray ionization mode and multiple-reaction monitoring( MRM)and quantitatived by external standard method.The results showed that the double purification effectively reduce the matrix interferences in liver.The standard calibration curve showed good linear behavior in the range from 5. 0 to 100. 0 μg/L and the relative coefficient was more than 0. 999.The limit of detection and the limit of quantitation of the method were 2. 0 μg/kg and 5. 0 μg/kg respectively.The spiked recoveries were 78. 6% to 90. 3%.The method is sensitive and accurate,which can be met the demands of quantitative analysis of vancomycin and norvancomycin in animal liver.
To establish a method for the determination of vancomycin and norvancomycin residue in animal liver based on Qu EChERS-SPE by ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS). The samples were extracted with mixed solution of 0. 1% formic acid and acetonitrile,purified first by PSA and C_(18),then cleaned with solid phase extraction( Strata-X-C),determined by UPLC-MS/MS with positive electrospray ionization mode and multiple-reaction monitoring( MRM)and quantitatived by external standard method.The results showed that the double purification effectively reduce the matrix interferences in liver.The standard calibration curve showed good linear behavior in the range from 5. 0 to 100. 0 μg/L and the relative coefficient was more than 0. 999.The limit of detection and the limit of quantitation of the method were 2. 0 μg/kg and 5. 0 μg/kg respectively.The spiked recoveries were 78. 6% to 90. 3%.The method is sensitive and accurate,which can be met the demands of quantitative analysis of vancomycin and norvancomycin in animal liver.
引文
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[2]韩峰,杨光昕,张璇,等.万古霉素和去甲万古霉素检测方法研究进展[J].食品安全质量检测学报,2017,8(9):3 414-3 419.
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[4]陆晓凤,吴建祥,徐少毅,等.万古霉素治疗医院获得性耐甲氧西林金黄色葡萄球菌肺炎的临床评价[J].中国感染与化疗杂志,2015,15(3):214-216.
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[7]刘佳佳,金芬,佘永新,等.液相色谱-串联质谱法测定牛奶中5种多肽类抗生素[J].分析化学,2011,39(5):652-657.
[8]李享,王玮,檀笑昕,等.毛细管电泳化学发光法测定人血清中的万古霉素和去甲万古霉素[J].分析试验室,2017,36(2):138-142.
[9]戴婷婷,蒋跃平,宋柏力,等.高效液相色谱法检测脑脊液中万古霉素药物浓度方法学建[J].中国医院药学杂志,2017,37(17):1 706-1 708.
[10]綦艳,李锦清,黄翠莉,等.超高效液相色谱-串联质谱法测定动物源性食品中万古霉素和去甲万古霉素的残留量[J].食品安全质量检测学报,2016,7(12):4 759-4 765.
[11]卢剑,范素芳,李强,等.高效液相色谱-串联质谱测定猪肉中万古霉素,去甲万古霉素和替考拉宁[J].食品科学,2016,37(10):193-197.
[12]冼燕萍,陈立伟,罗海英,等.UPLC-MS/MS法测定猪肉中万古霉素与去甲万古霉素[J].分析测试学报,2013,32(2):162-167.
[13]薛婷婷,黄冬梅,娄晓祎,等.双固相萃取/高效液相色谱-串联质谱法测定鱼类中糖肽类生素残留量[J].分析试验室,2018,37(1):36-39.
[14]薛婷婷,黄冬梅,严敏鸣,等.高效液相色谱-串联质谱法测定虾中万古霉素及去甲万古霉素残留量[J].分析测试学报,2017,36(6):773-777.
[15]彭丽,班付国,张发旺,等.超高效液相色谱-串联质谱法测定饲料中的万古霉素[J].中国畜牧兽医,2013,40(11):74-78.
[16]綦艳,李锦清,赵明桥,等.固相萃取/超高效液相色谱-串联质谱法测定乳与乳制品中万古霉素、去甲万古霉素残留[J].分析测试学报,2013,32(6):768-771.
[17]康明芹,胡婷婷,张勋,等.固相萃取-高效液相色谱-串联质谱法测定鲜人参中吲哚乙酸和吲哚丁酸[J].化学试剂,2016,38(7):641-643.
[18]胡贵祥,夏祥,朱惠芳.QuChERS在线凝胶色谱-气相色谱/质谱联用法测定水果蔬菜中氟虫腈农药残留[J].化学试剂,2017,39(5):509-512.
[19]ANASTASSIADES M,LEHOTAY S J,STAAIJNBAHER D,et al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and“dispersive solidphase extraction”for the determination of pesticide residues in produce[J]. J. AOAC Int.,2003,86(2):412-431.
[2]韩峰,杨光昕,张璇,等.万古霉素和去甲万古霉素检测方法研究进展[J].食品安全质量检测学报,2017,8(9):3 414-3 419.
[3]HAGIHARA M,CHIRISTINA S,DAVID P N. Development of HPLC methods for the determination of vancomycin in human plasma,mouse serum and bronchoalveolar lavage fluid[J]. J. Chromatogr. Sci.,2012,51(3):201-207.
[4]陆晓凤,吴建祥,徐少毅,等.万古霉素治疗医院获得性耐甲氧西林金黄色葡萄球菌肺炎的临床评价[J].中国感染与化疗杂志,2015,15(3):214-216.
[5]中华人民共和国农业部公告第560号[EB/OL].(2005-10-28)[2005-11-01]. http://www. moa. gov. cn/zwllm/tzgg/gg/200511/t20051117_496523.htm.
[6]食品中可能违法添加的非食用物质和易滥用的食品添加剂名单(第1~5批汇总)[EB/OL].(2011-04-19)[2011-04-22]. http://www. nhfpc. gov. cn/sps/s7892/201406/38e5c8a53615486888d93ed05ac9731a.shtml.
[7]刘佳佳,金芬,佘永新,等.液相色谱-串联质谱法测定牛奶中5种多肽类抗生素[J].分析化学,2011,39(5):652-657.
[8]李享,王玮,檀笑昕,等.毛细管电泳化学发光法测定人血清中的万古霉素和去甲万古霉素[J].分析试验室,2017,36(2):138-142.
[9]戴婷婷,蒋跃平,宋柏力,等.高效液相色谱法检测脑脊液中万古霉素药物浓度方法学建[J].中国医院药学杂志,2017,37(17):1 706-1 708.
[10]綦艳,李锦清,黄翠莉,等.超高效液相色谱-串联质谱法测定动物源性食品中万古霉素和去甲万古霉素的残留量[J].食品安全质量检测学报,2016,7(12):4 759-4 765.
[11]卢剑,范素芳,李强,等.高效液相色谱-串联质谱测定猪肉中万古霉素,去甲万古霉素和替考拉宁[J].食品科学,2016,37(10):193-197.
[12]冼燕萍,陈立伟,罗海英,等.UPLC-MS/MS法测定猪肉中万古霉素与去甲万古霉素[J].分析测试学报,2013,32(2):162-167.
[13]薛婷婷,黄冬梅,娄晓祎,等.双固相萃取/高效液相色谱-串联质谱法测定鱼类中糖肽类生素残留量[J].分析试验室,2018,37(1):36-39.
[14]薛婷婷,黄冬梅,严敏鸣,等.高效液相色谱-串联质谱法测定虾中万古霉素及去甲万古霉素残留量[J].分析测试学报,2017,36(6):773-777.
[15]彭丽,班付国,张发旺,等.超高效液相色谱-串联质谱法测定饲料中的万古霉素[J].中国畜牧兽医,2013,40(11):74-78.
[16]綦艳,李锦清,赵明桥,等.固相萃取/超高效液相色谱-串联质谱法测定乳与乳制品中万古霉素、去甲万古霉素残留[J].分析测试学报,2013,32(6):768-771.
[17]康明芹,胡婷婷,张勋,等.固相萃取-高效液相色谱-串联质谱法测定鲜人参中吲哚乙酸和吲哚丁酸[J].化学试剂,2016,38(7):641-643.
[18]胡贵祥,夏祥,朱惠芳.QuChERS在线凝胶色谱-气相色谱/质谱联用法测定水果蔬菜中氟虫腈农药残留[J].化学试剂,2017,39(5):509-512.
[19]ANASTASSIADES M,LEHOTAY S J,STAAIJNBAHER D,et al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and“dispersive solidphase extraction”for the determination of pesticide residues in produce[J]. J. AOAC Int.,2003,86(2):412-431.