干旱区生态环境知识资源中心(Arid): Simultaneous determination of 30 antibiotics in soil by ultra-high performance liquid chromatography-tandem mass spectrometry

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DOI	10.3724/SP.J.1123.2021.02019
	Simultaneous determination of 30 antibiotics in soil by ultra-high performance liquid chromatography-tandem mass spectrometry
	Hu Yu; Zhu Qingqing; Hu Ligang; Liao Chunyang
通讯作者	Liao, CY (corresponding author)，Chinese Acad Sci, Res Ctr Ecoenvironm Sci, State Key Lab Environm Chem & Ecotoxicol, Beijing 100085, Peoples R China. ; Liao, CY (corresponding author)，Univ Chinese Acad Sci UCAS, Coll Resources & Environm, Beijing 100049, Peoples R China. ; Liao, CY (corresponding author)，UCAS, Hangzhou Inst Adv Study, Inst Environm & Hlth, Hangzhou 310000, Peoples R China.
来源期刊	CHINESE JOURNAL OF CHROMATOGRAPHY
ISSN	1000-8713
出版年	2021
卷号	39 期号:8
英文摘要	The complexity of the soil matrix, as well as the wide spectrum and trace levels of antibiotic residues in soil, make highly sensitive instrumental methods, efficient purification and enrichment methods, and simultaneous determination of multiple antibiotics key and challenging aspects in the analysis of antibiotics in soil. In this study, a solid phase extraction-ultrahigh performance liquid chromatography-tandem mass spectrometry (SPE-UHPLC-MS/MS) method was developed for the simultaneous determination of 30 antibiotics (grouped into seven categories sulfonamides, fluoroquinolones, tetracyclines, macrolides, beta-lactams, amphenicols and lincosamides) in soil samples. In the UHPLC-MS/MS experiment, florfenicol and chloramphenicol were analyzed in the negative ionization multiple-reaction monitoring (MRM) mode, and the other 28 target analytes were analyzed in the positive MRM mode. Sensitive MS conditions were realized by optimizing the instrumental parameters such as collision energy and declustering potential. The effects of the injection solvent (proportion of methanol to water) and mobile phase (types and compositions of the solvents) on the shape and intensity of the chromatographic peaks were studied. The optimized UHPLC conditions were as follows: injection solvent, 10% (v/v) methanol aqueous solution; chromatographic column, BEH-C18 column; mobile phase, methanol and water both containing 0.1% (v/v) formic acid; flow rate, 0.4 mL/min; sample injection volume, 5.0 mu L. The effects of the extraction solution (the types and compositions of solvents) and clean-up processes (pH of the loading solution, as well as the types and compositions of the rinse solution and elution solvent) on the method performance were investigated. The acetonitrile/Na(2)EDTA-Mcllvaine buffer showed better extraction efficiency for fluoroquinolones than did the methanol/Na(2)EDTA-McIlvaine buffer. Improved recoveries of sulfonamides, macrolides, tetracyclines, and beta-lactams were observed when the pH of the loading solution was set to 8. 0. The recoveries of sulfadiazine and amoxicillin increased with a decrease in the proportion of methanol to water for the rinse solution. Compared to individual methanol or acetonitrile, the methanol-acetonitrile (1 :1, v/v) mixture showed better elution efficiency for the target analytes. The optimized pretreatment conditions were determined as follows: the soil sample was spiked with mixed internal standards, and then extracted with 10 mL of acetonitrile/Na(2)EDTA-McIlvaine buffer (1 :1, v/v) by shaking for 30 min and ultrasonication for 15 min. The extraction was repeated three times. The sample extract was adjusted to pH 8. 0 and loaded onto an Oasis HLB cartridge for purification. The cartridge was rinsed with 10 mL of water to remove impurities and eluted with 10 mL of methanol-acetonitrile (1 1, v/v). Quantitative analysis was conducted using the isotope internal standard method. The method limits of detection and quantification were in the range of 0. 013-1. 21 and 0. 043-4. 04 g/kg, respectively. The correlation coefficients of the calibration curve were 0. 992-1. 00, suggesting good linearity of the method. At three spiked levels (20, 100, and 200 g/kg), the average recoveries of most target antibiotics were 44. 8% to 164%, and the relative standard deviations were 0. 700% to 14. 8%. The method was successfully applied to the analysis of the 30 antibiotics in six soil samples. Seventeen antibiotics were detected in the soil samples, and the total contents of the antibiotics in each sample ranged from 73. 4 to 184 g/kg. Twelve antibiotics with a detection frequency of 100% included roxithromycin, clarithromycin, ciprofloxacin, norfloxacin, enrofloxacin, ofloxacin, fleroxacin, lomefloxacin, oxytetracycline, doxycycline, tetracycline, and penicillin G. Ciprofloxacin and norfloxacin were the predominant antibiotics in the soils, with contents in the range of 13. 7-32. 1 and 15. 6-43. 6 g/kg, respectively.
英文关键词	ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) solid phase extraction (SPE) antibiotics soil
类型	Article
语种	中文
收录类别	ESCI
WOS记录号	WOS:000753604700011
WOS关键词	BETA-LACTAM ANTIBIOTICS ; VETERINARY ANTIBIOTICS ; WASTE-WATER ; RESISTANCE GENES ; AGRICULTURAL SOILS ; SWINE MANURE ; HUMAN PLASMA ; AMOXICILLIN ; GREENHOUSE ; MATRICES
WOS类目	Chemistry, Analytical
WOS研究方向	Chemistry
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/376103
作者单位	[Hu Yu; Zhu Qingqing; Hu Ligang; Liao Chunyang] Chinese Acad Sci, Res Ctr Ecoenvironm Sci, State Key Lab Environm Chem & Ecotoxicol, Beijing 100085, Peoples R China; [Hu Yu; Zhu Qingqing; Hu Ligang; Liao Chunyang] Univ Chinese Acad Sci UCAS, Coll Resources & Environm, Beijing 100049, Peoples R China; [Liao Chunyang] UCAS, Hangzhou Inst Adv Study, Inst Environm & Hlth, Hangzhou 310000, Peoples R China
推荐引用方式 GB/T 7714	Hu Yu,Zhu Qingqing,Hu Ligang,et al. Simultaneous determination of 30 antibiotics in soil by ultra-high performance liquid chromatography-tandem mass spectrometry[J],2021,39(8).
APA	Hu Yu,Zhu Qingqing,Hu Ligang,&Liao Chunyang.(2021).Simultaneous determination of 30 antibiotics in soil by ultra-high performance liquid chromatography-tandem mass spectrometry.CHINESE JOURNAL OF CHROMATOGRAPHY,39(8).
MLA	Hu Yu,et al."Simultaneous determination of 30 antibiotics in soil by ultra-high performance liquid chromatography-tandem mass spectrometry".CHINESE JOURNAL OF CHROMATOGRAPHY 39.8(2021).