QuEChERS/超高效液相色谱-串联质谱法快速测定土壤中19种氟喹诺酮类抗生素残留
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摘要
建立了一种基于QuEChERS前处理技术,结合超高效液相色谱-串联质谱(UPLC-MS/MS)和内标法,快速测定土壤中19种氟喹诺酮类抗生素(FQs)残留的分析方法。5. 0 g土壤样品添加200μg/kg基质匹配同位素内标后,经20 m L 0. 1 mol/L EDTA-McIlvaine缓冲液和乙腈混合溶剂(体积比1∶1)提取,基质分散固相萃取(150 mg无水MgSO4、15 mg PSA、15 mg C18)净化后,采用UPLC-MS/MS进行测定。质谱分析采用电喷雾电离,正离子扫描,多反应监测模式。在优化条件下,19种抗生素的相关系数(r~2)为0. 992～0. 998,检出限为0. 2～1. 0μg/kg,定量下限为1. 0～5. 0μg/kg;在10、50、200μg/kg加标水平下的回收率为65. 2%～104%,相对标准偏差(n=5)不大于14%。该方法操作简单快速、准确度高,适用于土壤中氟喹诺酮类抗生素残留的检测。
A method of ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS) combined with internal standard method was developed for the simultaneous determination of19 kinds of fluoroquinolones antibiotic( FQs) residues in soil based on QuEChERS( Quick,Easy,Cheap,Effective,Rugged,Safe) pre-treatment. Firstly,5. 0 g of soil was blended with 100 μL 10 mg/L internal standard compounds,then the analyte was extracted with 20 m L 0. 1 mol/L EDTA-McIlvaine buffer and acetonitrile( 1 ∶ 1,by volume),cleaned-up with a matrix dispersive solid phase extraction material( 150 mg anhydrous MgSO4,15 mg PSA,15 mg C18),finally detected by UPLC-MS/MS with electrospray ionization in positive ion scanning under multiple reaction monitoring mode. Under the optimized conditions,the limits of detection and quantitation of the method were in the ranges of 0. 2-1. 0 μg/kg and 1. 0-5. 0 μg/kg,respectively,with correlation coefficients( r~2) of 0. 992-0. 998. Recoveries for 19 FQs at three spiked levels of 10,50 and 200 μg/kg ranged from 65. 2% to 104% with relative standard deviations( n = 5) not more than 14%. The method was simple,rapid and accurate,and was suitable for the determination of fluoroquinolones antibiotic residues in soil.
A method of ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS) combined with internal standard method was developed for the simultaneous determination of19 kinds of fluoroquinolones antibiotic( FQs) residues in soil based on QuEChERS( Quick,Easy,Cheap,Effective,Rugged,Safe) pre-treatment. Firstly,5. 0 g of soil was blended with 100 μL 10 mg/L internal standard compounds,then the analyte was extracted with 20 m L 0. 1 mol/L EDTA-McIlvaine buffer and acetonitrile( 1 ∶ 1,by volume),cleaned-up with a matrix dispersive solid phase extraction material( 150 mg anhydrous MgSO4,15 mg PSA,15 mg C18),finally detected by UPLC-MS/MS with electrospray ionization in positive ion scanning under multiple reaction monitoring mode. Under the optimized conditions,the limits of detection and quantitation of the method were in the ranges of 0. 2-1. 0 μg/kg and 1. 0-5. 0 μg/kg,respectively,with correlation coefficients( r~2) of 0. 992-0. 998. Recoveries for 19 FQs at three spiked levels of 10,50 and 200 μg/kg ranged from 65. 2% to 104% with relative standard deviations( n = 5) not more than 14%. The method was simple,rapid and accurate,and was suitable for the determination of fluoroquinolones antibiotic residues in soil.
引文
[1] Dai X H,Xue Y G,Liu H J,Dai L L,Yan H,Li N. Environ. Sci.(戴晓虎,薛勇刚,刘华杰,戴翎翎,严寒,李宁.环境科学),2016,37(4):1553-1561.
[2] Gao J H,Xie X Y,Zhang H Y,Zhu J M,Xie C R,Wang Z W. J. Lanzhou Univ.:Nat. Sci. Ed.(高俊红,谢晓芸,张涵瑜,朱俊民,谢超然,王兆炜.兰州大学学报:自然科学版),2016,52(5):593-598.
[3] Fadário Frade V M,Dias M,Silva Costa Teixeira A C,Alves Palma M S. Bra. J. Pharm. Sci.,2014,50(1):41-54.
[4] Zhang X,Xiang L,Mo C H,Li Y W,Cai Q Y,Huang X P,Wu X L,Li H. J. Agro-Environ. Sci.(张旭,向垒,莫测辉,李彦文,蔡全英,黄献培,吴小莲,李慧.农业环境科学学报),2014,33(7):1345-1350.
[5] Riaz L,Mahmood T,Khalid A,Rashid A,Ahmed Siddique M B,Kamal A,Coyne M S. Chemosphere,2018,191:704-720.
[6] Peruchi L M,Fostier A H,Rath S. Chemosphere,2015,119:310-317.
[7] Zhao F K,Yang L,Qiao M,Li S J,Sun L. Soils(赵方凯,杨磊,乔敏,李守娟,孙龙.土壤),2017,49(3):428-436.
[8] Wei R C,Ge F,Zhang L L,Hou X,Cao Y N,Gong L,Chen M,Wang R,Bao E D. Chemosphere,2016,144:2377-2383.
[9] Li X W,Xie Y F,Li C L,Zhao H N,Zhao H,Wang N,Wang J F. Sci. Total Environ.,2014,468/469:258-264.
[10] Wen C H,Lin S L,Fuh M R. Talanta,2017,164:85-91.
[11] Bruzzoniti M C,Checchini L,De Carlo R M,Orlandini S,Rivoira L,Del Bubba M. Anal. Bioanal. Chem.,2014,406:4089-4116.
[12] Guo C N,Wang M R,Xiao H,Huai B B,Wang F,Pan G F,Liao X P,Liu Y H. J. Chromatogr. B,2016,1027:110-118.
[13] Li X W,Guo P,Shan Y W,Ke Y B,Li H,Fu Q,Wang Y Y,Liu T H,Xia X. J. Chromatogr. A,2017,1499:57-64.
[14] Zhao Z Y,Zhang Y M,Xuan Y F,Song W,Si W S,Zhao Z H,Rao Q X. J. Chromatogr. B,2016,1022:281-289.
[15] Wang J M,Liu Y P,Chen J,Wu H Z,Xia W,Li Z G,Qian M R. J. Instrum. Anal.(汪建妹,刘艳平,陈静,吴慧珍,夏魏,李祖光,钱鸣蓉.分析测试学报),2017,36(2):218-223.
[16] Meng M H,He Z Y,Xu Y P,Wang L,Peng Y,Liu X W. J. Agro-Environ. Sci.(孟明辉,贺泽英,徐亚平,王璐,彭祎,刘潇威.农业环境科学学报),2017,36(8):1672-1679.
[17] GB/T 27404-2008. Criterion on Quality Control of Laboratories-Chemical Testing of Food. National Standards of thePeople's Republic of China(实验室质量控制规范食品理化检测.中华人民共和国国家标准).
[18] Sun J T,Zeng Q T,Tsang D C W,Zhu L Z,Li X D. Chemosphere,2017,189:301-308.
[19] Zhao J,Bi C J,Chen Z L,Shi Q,Li L R,Yao C X. J. Ecol. Rural Environ.(赵晶,毕春娟,陈振楼,施庆,李林茹,姚春霞.生态与农村环境学报),2017,33(2):120-126.
[2] Gao J H,Xie X Y,Zhang H Y,Zhu J M,Xie C R,Wang Z W. J. Lanzhou Univ.:Nat. Sci. Ed.(高俊红,谢晓芸,张涵瑜,朱俊民,谢超然,王兆炜.兰州大学学报:自然科学版),2016,52(5):593-598.
[3] Fadário Frade V M,Dias M,Silva Costa Teixeira A C,Alves Palma M S. Bra. J. Pharm. Sci.,2014,50(1):41-54.
[4] Zhang X,Xiang L,Mo C H,Li Y W,Cai Q Y,Huang X P,Wu X L,Li H. J. Agro-Environ. Sci.(张旭,向垒,莫测辉,李彦文,蔡全英,黄献培,吴小莲,李慧.农业环境科学学报),2014,33(7):1345-1350.
[5] Riaz L,Mahmood T,Khalid A,Rashid A,Ahmed Siddique M B,Kamal A,Coyne M S. Chemosphere,2018,191:704-720.
[6] Peruchi L M,Fostier A H,Rath S. Chemosphere,2015,119:310-317.
[7] Zhao F K,Yang L,Qiao M,Li S J,Sun L. Soils(赵方凯,杨磊,乔敏,李守娟,孙龙.土壤),2017,49(3):428-436.
[8] Wei R C,Ge F,Zhang L L,Hou X,Cao Y N,Gong L,Chen M,Wang R,Bao E D. Chemosphere,2016,144:2377-2383.
[9] Li X W,Xie Y F,Li C L,Zhao H N,Zhao H,Wang N,Wang J F. Sci. Total Environ.,2014,468/469:258-264.
[10] Wen C H,Lin S L,Fuh M R. Talanta,2017,164:85-91.
[11] Bruzzoniti M C,Checchini L,De Carlo R M,Orlandini S,Rivoira L,Del Bubba M. Anal. Bioanal. Chem.,2014,406:4089-4116.
[12] Guo C N,Wang M R,Xiao H,Huai B B,Wang F,Pan G F,Liao X P,Liu Y H. J. Chromatogr. B,2016,1027:110-118.
[13] Li X W,Guo P,Shan Y W,Ke Y B,Li H,Fu Q,Wang Y Y,Liu T H,Xia X. J. Chromatogr. A,2017,1499:57-64.
[14] Zhao Z Y,Zhang Y M,Xuan Y F,Song W,Si W S,Zhao Z H,Rao Q X. J. Chromatogr. B,2016,1022:281-289.
[15] Wang J M,Liu Y P,Chen J,Wu H Z,Xia W,Li Z G,Qian M R. J. Instrum. Anal.(汪建妹,刘艳平,陈静,吴慧珍,夏魏,李祖光,钱鸣蓉.分析测试学报),2017,36(2):218-223.
[16] Meng M H,He Z Y,Xu Y P,Wang L,Peng Y,Liu X W. J. Agro-Environ. Sci.(孟明辉,贺泽英,徐亚平,王璐,彭祎,刘潇威.农业环境科学学报),2017,36(8):1672-1679.
[17] GB/T 27404-2008. Criterion on Quality Control of Laboratories-Chemical Testing of Food. National Standards of thePeople's Republic of China(实验室质量控制规范食品理化检测.中华人民共和国国家标准).
[18] Sun J T,Zeng Q T,Tsang D C W,Zhu L Z,Li X D. Chemosphere,2017,189:301-308.
[19] Zhao J,Bi C J,Chen Z L,Shi Q,Li L R,Yao C X. J. Ecol. Rural Environ.(赵晶,毕春娟,陈振楼,施庆,李林茹,姚春霞.生态与农村环境学报),2017,33(2):120-126.
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