Fe_3O_4@SiO_2@SDS的制备及其在氟喹诺酮检测中的应用
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摘要
制备了Fe_3O_4@SiO_2@SDS磁性混合半胶束固相萃取吸附剂,并结合高效液相色谱法,分析检测了环境水体中的痕量氟喹诺酮类抗生素(FQs).考察了Fe_3O_4@SiO_2用量、SDS用量、p H值、乙腈中醋酸量等因素对萃取效果的影响.结果表明,在优化的试验条件下,100 m L水样中加入30 mgFe_3O_4@SiO_2和100 mg SDS可以实现6种FQs(左氧氟沙星、环丙沙星、洛美沙星、恩诺沙星、加替沙星和司帕沙星)的快速吸附,吸附效率分别为87%,82%,80%,97%,85%,84%,富集倍数达到40～77.结合高效液相色谱法检测,方法检出限为0. 1 ng·mL~(-1),可以实现痕量分析,并成功地应用于实际水样分析,回收率为87%～120%.可见,Fe3O4@Si O2@SDS混合半胶束固相萃取吸附剂具有萃取效率高、操作简单、绿色环保等优点,是一种有效的样品前处理技术.
Based on high performance liquid chromatography( HPLC),the mixed hemi/ad-micellesmagnetic nanoparticles Fe_3O_4@SiO_2@ SDS was prepared to extract the trace quantities of some fluoroquinolones( FQs). The effects of Fe_3O_4@SiO_2,SDS,pH and HAc on the extraction effect were investigated. The results show that under the optimum conditions with pH value of 4,Fe_3O_4@SiO_2 amount of 30 mg and SDS amount of 100 mg,six FQ drugs of levofloxacin,ciprofloxacin,lomefloxacin,enrofloxacin,gatifloxacin and sparfloxacin can be absorbed rapidly from 100 m L water, and the adsorption efficiencies are 87%,82%,80%,97%,85% and 84%,respectively. The enrichment multiple reaches 40 to 77,and the detection limit is 0. 1 ng·mL~(-1). The trace analysis is achieved and successfully applied to actual water sample analysis with recovery rate of 87% to 120% by HPLC. The SDS-coated Fe_3O_4@SiO_2 magnetic micelle hybrid solid phase extraction is an effective sample for pretreatment technology with efficient,simple and green advantages.
Based on high performance liquid chromatography( HPLC),the mixed hemi/ad-micellesmagnetic nanoparticles Fe_3O_4@SiO_2@ SDS was prepared to extract the trace quantities of some fluoroquinolones( FQs). The effects of Fe_3O_4@SiO_2,SDS,pH and HAc on the extraction effect were investigated. The results show that under the optimum conditions with pH value of 4,Fe_3O_4@SiO_2 amount of 30 mg and SDS amount of 100 mg,six FQ drugs of levofloxacin,ciprofloxacin,lomefloxacin,enrofloxacin,gatifloxacin and sparfloxacin can be absorbed rapidly from 100 m L water, and the adsorption efficiencies are 87%,82%,80%,97%,85% and 84%,respectively. The enrichment multiple reaches 40 to 77,and the detection limit is 0. 1 ng·mL~(-1). The trace analysis is achieved and successfully applied to actual water sample analysis with recovery rate of 87% to 120% by HPLC. The SDS-coated Fe_3O_4@SiO_2 magnetic micelle hybrid solid phase extraction is an effective sample for pretreatment technology with efficient,simple and green advantages.
引文
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[8]崔飞飞,乔显亮,罗翔,等.河口水体中溶解性物质对氟喹诺酮光解速率常数的影响[J].环境污染与防治,2016,38(11):79-83,89.CUI F F,QIAO X L,LUO X,et al.Influence of dissolved matters on the photodegradation rate constants of fluoroquinolones in estuary water[J].Environmental Pollution and Control,2016,38(11):79-83,89.(in Chinese)
[9]MUTAVDIC'PAVLOVIC'D,NIKIC'K,LIVAZOVIC'S,et al.Preparation and application of sulfaguanidineimprinted polymer on solid-phase extraction of pharmaceuticals from water[J].Talanta,2015,131(1):99-107.
[10]FARZANEH S,LISH A B,ABDOUSS M,et al.Molecularly imprinted polymer nanoparticles for olanzapine recognition:application for solid phase extraction and sustained release[J].RSC Advances,2015,5(12):9154-9166.
[11]ZHANG H Y,WEI Y W,ZHOU J H,et al.Preparation and application of a molecular imprinting matrix solid phase dispersion extraction for the determination of olaquindox in chicken by high performance liquid chromatography[J].Food Analytical Methods,2013,6(3):915-921.
[12]RAMOS-PAYN M,VILLAR-NAVARRO M,FER-NNDEZ-TORRES R,et al.Electromembrane extraction(EME)-an easy,novel and rapid extraction procedure for the HPLC determination of fluoroquinolones in wastewater samples[J].Analytical and Bioanalytical Chemistry,2013,405(8):2575-2584.
[2]PEREIRA ANDRM P T,SILVA L J G,MEISEL LM,et al.Fluoroquinolones and tetracycline antibiotics in a portuguese aquaculture system and aquatic surroundings:occurrence and environmental impact[J].Journal of Toxicology and Environmental Health,Part A,2015,78(15):959-975.
[3]韦笑,孔祥吉,单正军.高效液相色谱法测定稻田土壤中环吡氟草酮残留[J].分析实验室,2018,37(2):197-201.WEI X,KONG X J,SHAN Z J.Study on residue analysis of flufenacet in rice soil[J].Chinese Journal of Analysis Laboratory,2018,37(2):197-201.(in Chinese)
[4]于永,王新.氟喹诺酮类兽药残留分析方法的综述[J].现代畜牧科技,2014(4):251-252.YU Y,WANG X.Review of analytical methods for residue of fluoroquinolones veterinary drug[J].Modern Animal Husbandry Science&Technology,2014(4):251-252.(in Chinese)
[5]WANG H,ZHAO X L,MENG W,et al.Cetyltrimethylammonium bromide-coated Fe3O4magnetic nanoparticles for rapid analysis of 15 trace polycyclic aromatic hydrocarbons in aquatic environments by UPLC-FLD[J].Analytical Chemistry,2015,87(15):7667-7675.
[6]ZHANG Z,LIU J F,FENG T T,et al.Time-resolved fluoroimmunoassay as an advantageous analytical method for assessing the total concentration and environmental risk of fluoroquinolones in surface waters[J].Environmental Science&Technology,2013,47(1):454-462.
[7]BEIRAGHI A,POURGHAZI K,AMOLI-DIVA M,et al.Magnetic solid phase extraction of mefenamic acid from biological samples based on the formation of mixed hemimicelle aggregates on Fe3O4nanoparticles prior to its HPLC-UV detection[J].Journal of Chromatography B,2014,945-946:46-52.
[8]崔飞飞,乔显亮,罗翔,等.河口水体中溶解性物质对氟喹诺酮光解速率常数的影响[J].环境污染与防治,2016,38(11):79-83,89.CUI F F,QIAO X L,LUO X,et al.Influence of dissolved matters on the photodegradation rate constants of fluoroquinolones in estuary water[J].Environmental Pollution and Control,2016,38(11):79-83,89.(in Chinese)
[9]MUTAVDIC'PAVLOVIC'D,NIKIC'K,LIVAZOVIC'S,et al.Preparation and application of sulfaguanidineimprinted polymer on solid-phase extraction of pharmaceuticals from water[J].Talanta,2015,131(1):99-107.
[10]FARZANEH S,LISH A B,ABDOUSS M,et al.Molecularly imprinted polymer nanoparticles for olanzapine recognition:application for solid phase extraction and sustained release[J].RSC Advances,2015,5(12):9154-9166.
[11]ZHANG H Y,WEI Y W,ZHOU J H,et al.Preparation and application of a molecular imprinting matrix solid phase dispersion extraction for the determination of olaquindox in chicken by high performance liquid chromatography[J].Food Analytical Methods,2013,6(3):915-921.
[12]RAMOS-PAYN M,VILLAR-NAVARRO M,FER-NNDEZ-TORRES R,et al.Electromembrane extraction(EME)-an easy,novel and rapid extraction procedure for the HPLC determination of fluoroquinolones in wastewater samples[J].Analytical and Bioanalytical Chemistry,2013,405(8):2575-2584.
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