PMID- 27311954 OWN - NLM STAT- MEDLINE DCOM- 20180118 LR - 20191210 IS - 1618-2650 (Electronic) IS - 1618-2642 (Linking) VI - 408 IP - 21 DP - 2016 Aug TI - Multiplug filtration cleanup method with multi-walled carbon nanotubes for the analysis of malachite green, diethylstilbestrol residues, and their metabolites in aquatic products by liquid chromatography-tandem mass spectrometry. PG - 5801-5809 LID - 10.1007/s00216-016-9686-6 [doi] AB - The food safety supervision in aquatic products has raised public concern in recent years. In this study, a liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method for the simultaneous quantification and identification of four residues of the ever widely used analytes (including malachite green, leucomalachite green, diethylstilbestrol, and dienestrol) in aquaculture samples was developed. For sample preparation, a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used, which was initially developed for pesticide residue analysis. For cleanup procedure, low-temperature cleanup method was combined with multiplug filtration cleanup (m-PFC) method based on multi-walled carbon nanotubes (MWCNTs). The volume of water, extraction solvent, cleanup sorbents, and m-PFC procedure were optimized for carp, striped bass, and giant salamander matrices. It was validated by analyzing four residues in each matrix spiked at three concentration levels of 0.5, 5, and 50 mug/kg (n = 5). The method was successfully validated according to the 2002/657/EC guidelines. After optimization, spike recoveries were within 73-106 % and <15 % relative standard deviations (RSDs) for all analytes in the tested matrices. Limits of quantification (LOQs) for the proposed method ranged from 0.10 to 0.50 mug/kg. Matrix-matched calibrations were performed with the coefficients of determination >0.998 between concentration levels of 0.5 and 200 mug/kg. The developed method was successfully applied to the determination of residues in market samples. Graphical abstract Flow chart of multi-plug filtration cleanup combined with low-temperature cleanup method. FAU - Qin, Yuhong AU - Qin Y AD - Beijing Advanced Innovation Center for Food Nutrition and Human Health, Department of Applied Chemistry, College of Science, China Agricultural University, No. 2 Yuanmingyuan West Road, Beijing, 100193, China. FAU - Zhang, Jingru AU - Zhang J AD - Beijing Advanced Innovation Center for Food Nutrition and Human Health, Department of Applied Chemistry, College of Science, China Agricultural University, No. 2 Yuanmingyuan West Road, Beijing, 100193, China. FAU - Li, Yanjie AU - Li Y AD - Beijing Advanced Innovation Center for Food Nutrition and Human Health, Department of Applied Chemistry, College of Science, China Agricultural University, No. 2 Yuanmingyuan West Road, Beijing, 100193, China. FAU - Han, Yongtao AU - Han Y AD - Beijing Advanced Innovation Center for Food Nutrition and Human Health, Department of Applied Chemistry, College of Science, China Agricultural University, No. 2 Yuanmingyuan West Road, Beijing, 100193, China. FAU - Zou, Nan AU - Zou N AD - Beijing Advanced Innovation Center for Food Nutrition and Human Health, Department of Applied Chemistry, College of Science, China Agricultural University, No. 2 Yuanmingyuan West Road, Beijing, 100193, China. FAU - Jiang, Yanbin AU - Jiang Y AD - China Animal Disease Control Center (CADC), Maizidian Street Building 20, Beijing, 100125, China. FAU - Shan, Jihao AU - Shan J AD - Institute of Agro-Products Processing Science & Technology, Chinese Academy of Agricultural Sciences (CAAS), No. 2 Yuanmingyuan West Road, Haidian District, Beijing, 100193, China. FAU - Pan, Canping AU - Pan C AD - Beijing Advanced Innovation Center for Food Nutrition and Human Health, Department of Applied Chemistry, College of Science, China Agricultural University, No. 2 Yuanmingyuan West Road, Beijing, 100193, China. canpingp@cau.edu.cn. LA - eng PT - Journal Article PT - Validation Study DEP - 20160616 PL - Germany TA - Anal Bioanal Chem JT - Analytical and bioanalytical chemistry JID - 101134327 RN - 0 (Nanotubes, Carbon) RN - 0 (Rosaniline Dyes) RN - 12058M7ORO (malachite green) RN - 731DCA35BT (Diethylstilbestrol) RN - 8U61G37Z20 (leucomalachite green) RN - RRW32X4U1F (Dienestrol) SB - IM MH - Animals MH - Bass/metabolism MH - Carps/metabolism MH - Chromatography, Liquid/methods MH - Dienestrol/analysis/metabolism MH - Diethylstilbestrol/*analysis/metabolism MH - Drug Residues/*analysis/metabolism MH - Food Contamination/*analysis MH - Limit of Detection MH - Nanotubes, Carbon/*chemistry MH - Rosaniline Dyes/*analysis/metabolism MH - Seafood/*analysis MH - Solid Phase Extraction/methods MH - Tandem Mass Spectrometry/*methods MH - Urodela/metabolism OTO - NOTNLM OT - Aquaculture OT - Multiple-walled carbon nanotubes OT - Multiplug filtration cleanup OT - Residue analysis EDAT- 2016/06/18 06:00 MHDA- 2018/01/19 06:00 CRDT- 2016/06/18 06:00 PHST- 2016/05/02 00:00 [received] PHST- 2016/06/02 00:00 [accepted] PHST- 2016/05/22 00:00 [revised] PHST- 2016/06/18 06:00 [entrez] PHST- 2016/06/18 06:00 [pubmed] PHST- 2018/01/19 06:00 [medline] AID - 10.1007/s00216-016-9686-6 [pii] AID - 10.1007/s00216-016-9686-6 [doi] PST - ppublish SO - Anal Bioanal Chem. 2016 Aug;408(21):5801-5809. doi: 10.1007/s00216-016-9686-6. Epub 2016 Jun 16.