Evaluation of two modified quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation methods for the analysis of baclofen and gabapentin in feeds by liquid chromatography tandem mass spectrometry

•A LC–MS/MS method was firstly developed for baclofen and gabapentin in feeds.•Two QuEChERS sample preparation methods had been developed and compared.•Selectivity, linearity, trueness, precision, LOD and LOQ had been validated.•The whole method was fast, reliable, convenient and sensitive. This pap...

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Veröffentlicht in:Journal of pharmaceutical and biomedical analysis 2014-01, Vol.88, p.53-59
Hauptverfasser: Hou, Xiao-Lin, Wu, Yin-Liang, Chen, Ruo-Xia, Zhu, Yong, Lv, Yan, Xu, Xiu-Qin
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container_title Journal of pharmaceutical and biomedical analysis
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creator Hou, Xiao-Lin
Wu, Yin-Liang
Chen, Ruo-Xia
Zhu, Yong
Lv, Yan
Xu, Xiu-Qin
description •A LC–MS/MS method was firstly developed for baclofen and gabapentin in feeds.•Two QuEChERS sample preparation methods had been developed and compared.•Selectivity, linearity, trueness, precision, LOD and LOQ had been validated.•The whole method was fast, reliable, convenient and sensitive. This paper presents a new analytical method for the simultaneous determination of baclofen and gabapentin in feeds based on two modified quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation methods and liquid chromatography tandem mass spectrometry (LC–MS/MS). For the two modified QuEChERS methods, samples were first extracted with acidified acetonitrile (5.0% acetic acid, v/v) without using acetonitrile salting-out extraction. Then, the first modified QuEChERS method was established according to the original QuEChERS cleanup procedure. For the second modified QuEChERS method, the extract was evaporated to dryness and reconstituted in acetonitrile. Subsequently, the analytes in the reconstituted solution were retained by primary secondary amine (PSA) and released from PSA with 1.0% formic acid in methanol. Finally, the eluate was evaporated and dissolved in 0.1% formic acid solution/methanol (v/v, 80:20). All of the samples were analyzed by LC–MS/MS on a Waters Acquity BEH C18 column with 0.1% formic acid in water/methanol as the mobile phase with gradient elution. The matrix effect, recovery, and repeatability, within laboratory reproducibility, and the LODs and LOQs of the two modified QuEChERS sample preparation methods were investigated and compared. Comparative results showed that the second method was obviously superior to the first method.
doi_str_mv 10.1016/j.jpba.2013.08.026
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This paper presents a new analytical method for the simultaneous determination of baclofen and gabapentin in feeds based on two modified quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation methods and liquid chromatography tandem mass spectrometry (LC–MS/MS). For the two modified QuEChERS methods, samples were first extracted with acidified acetonitrile (5.0% acetic acid, v/v) without using acetonitrile salting-out extraction. Then, the first modified QuEChERS method was established according to the original QuEChERS cleanup procedure. For the second modified QuEChERS method, the extract was evaporated to dryness and reconstituted in acetonitrile. Subsequently, the analytes in the reconstituted solution were retained by primary secondary amine (PSA) and released from PSA with 1.0% formic acid in methanol. Finally, the eluate was evaporated and dissolved in 0.1% formic acid solution/methanol (v/v, 80:20). All of the samples were analyzed by LC–MS/MS on a Waters Acquity BEH C18 column with 0.1% formic acid in water/methanol as the mobile phase with gradient elution. The matrix effect, recovery, and repeatability, within laboratory reproducibility, and the LODs and LOQs of the two modified QuEChERS sample preparation methods were investigated and compared. 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This paper presents a new analytical method for the simultaneous determination of baclofen and gabapentin in feeds based on two modified quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation methods and liquid chromatography tandem mass spectrometry (LC–MS/MS). For the two modified QuEChERS methods, samples were first extracted with acidified acetonitrile (5.0% acetic acid, v/v) without using acetonitrile salting-out extraction. Then, the first modified QuEChERS method was established according to the original QuEChERS cleanup procedure. For the second modified QuEChERS method, the extract was evaporated to dryness and reconstituted in acetonitrile. Subsequently, the analytes in the reconstituted solution were retained by primary secondary amine (PSA) and released from PSA with 1.0% formic acid in methanol. Finally, the eluate was evaporated and dissolved in 0.1% formic acid solution/methanol (v/v, 80:20). All of the samples were analyzed by LC–MS/MS on a Waters Acquity BEH C18 column with 0.1% formic acid in water/methanol as the mobile phase with gradient elution. The matrix effect, recovery, and repeatability, within laboratory reproducibility, and the LODs and LOQs of the two modified QuEChERS sample preparation methods were investigated and compared. Comparative results showed that the second method was obviously superior to the first method.</description><subject>Acetonitriles - chemistry</subject><subject>Amines - analysis</subject><subject>Amines - chemistry</subject><subject>Animal Feed</subject><subject>Baclofen</subject><subject>Baclofen - analysis</subject><subject>Chemistry Techniques, Analytical</subject><subject>Chemistry, Pharmaceutical - methods</subject><subject>Chemistry, Pharmaceutical - standards</subject><subject>Chromatography, Liquid</subject><subject>Cyclohexanecarboxylic Acids - analysis</subject><subject>Excitatory Amino Acid Antagonists - analysis</subject><subject>Feed</subject><subject>Formates - chemistry</subject><subject>GABA-B Receptor Agonists - analysis</subject><subject>Gabapentin</subject><subject>gamma-Aminobutyric Acid - analysis</subject><subject>LC–MS/MS</subject><subject>Mass Spectrometry</subject><subject>Methanol - chemistry</subject><subject>QuEChERS</subject><subject>Reproducibility of Results</subject><subject>Time Factors</subject><subject>Water - chemistry</subject><issn>0731-7085</issn><issn>1873-264X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2014</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNp9UV2r1DAQLaJ416t_wAfJ4xW2a5J2mxZ8kWX9gAviF_gWpslkm7VtepN0pX_U32PWvfooBMIw55w5MyfLnjO6YZRVr46b49TChlNWbGi9obx6kK1YLYqcV-X3h9mKioLlgtbbq-xJCEdK6ZY15ePsipe0qIqKr7Jf-xP0M0TrRuIMiT8dGZy2xqImd7NVP9YEISxrojqEKRXGoIr2hGvi58MhoWDUJIBBcvNp3u-6_ecvL1M9TD2SyeME_iI-YOycDsQ4T2KHiQb9Emw4T21B9c7g-EfrAC1MOEY7kvQMYiK1C-ltsqOTDe8GiO7gYeoWEhMDBzJACCRMyVnqYvTL0-yRgT7gs_v_Ovv2dv919z6__fjuw-7Nba6KbRVzoJoJJhqhatbUolVMla0WVFMlFKTRRcOxZGXZUl4AZRy5EU1bt2wrRF3o4jq7uehO3t3NGKIcbFDY9zCim4NkZcVZXW0bmqD8AlXeheDRyMnbAfwiGZXnPOVRnvOU5zwlrWXKM5Fe3OvP7YD6H-VvgAnw-gLAtOXJopdBWRwVauvTOaR29n_6vwEBe7V7</recordid><startdate>20140125</startdate><enddate>20140125</enddate><creator>Hou, Xiao-Lin</creator><creator>Wu, Yin-Liang</creator><creator>Chen, Ruo-Xia</creator><creator>Zhu, Yong</creator><creator>Lv, Yan</creator><creator>Xu, Xiu-Qin</creator><general>Elsevier B.V</general><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7X8</scope></search><sort><creationdate>20140125</creationdate><title>Evaluation of two modified quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation methods for the analysis of baclofen and gabapentin in feeds by liquid chromatography tandem mass spectrometry</title><author>Hou, Xiao-Lin ; Wu, Yin-Liang ; Chen, Ruo-Xia ; Zhu, Yong ; Lv, Yan ; Xu, Xiu-Qin</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c356t-a0d171797c81987bc1c4bd70d0c7caeed392e4144b023a012e2f79b8b157783d3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2014</creationdate><topic>Acetonitriles - chemistry</topic><topic>Amines - analysis</topic><topic>Amines - chemistry</topic><topic>Animal Feed</topic><topic>Baclofen</topic><topic>Baclofen - analysis</topic><topic>Chemistry Techniques, Analytical</topic><topic>Chemistry, Pharmaceutical - methods</topic><topic>Chemistry, Pharmaceutical - standards</topic><topic>Chromatography, Liquid</topic><topic>Cyclohexanecarboxylic Acids - analysis</topic><topic>Excitatory Amino Acid Antagonists - analysis</topic><topic>Feed</topic><topic>Formates - chemistry</topic><topic>GABA-B Receptor Agonists - analysis</topic><topic>Gabapentin</topic><topic>gamma-Aminobutyric Acid - analysis</topic><topic>LC–MS/MS</topic><topic>Mass Spectrometry</topic><topic>Methanol - chemistry</topic><topic>QuEChERS</topic><topic>Reproducibility of Results</topic><topic>Time Factors</topic><topic>Water - chemistry</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Hou, Xiao-Lin</creatorcontrib><creatorcontrib>Wu, Yin-Liang</creatorcontrib><creatorcontrib>Chen, Ruo-Xia</creatorcontrib><creatorcontrib>Zhu, Yong</creatorcontrib><creatorcontrib>Lv, Yan</creatorcontrib><creatorcontrib>Xu, Xiu-Qin</creatorcontrib><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><jtitle>Journal of pharmaceutical and biomedical analysis</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Hou, Xiao-Lin</au><au>Wu, Yin-Liang</au><au>Chen, Ruo-Xia</au><au>Zhu, Yong</au><au>Lv, Yan</au><au>Xu, Xiu-Qin</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Evaluation of two modified quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation methods for the analysis of baclofen and gabapentin in feeds by liquid chromatography tandem mass spectrometry</atitle><jtitle>Journal of pharmaceutical and biomedical analysis</jtitle><addtitle>J Pharm Biomed Anal</addtitle><date>2014-01-25</date><risdate>2014</risdate><volume>88</volume><spage>53</spage><epage>59</epage><pages>53-59</pages><issn>0731-7085</issn><eissn>1873-264X</eissn><abstract>•A LC–MS/MS method was firstly developed for baclofen and gabapentin in feeds.•Two QuEChERS sample preparation methods had been developed and compared.•Selectivity, linearity, trueness, precision, LOD and LOQ had been validated.•The whole method was fast, reliable, convenient and sensitive. This paper presents a new analytical method for the simultaneous determination of baclofen and gabapentin in feeds based on two modified quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation methods and liquid chromatography tandem mass spectrometry (LC–MS/MS). For the two modified QuEChERS methods, samples were first extracted with acidified acetonitrile (5.0% acetic acid, v/v) without using acetonitrile salting-out extraction. Then, the first modified QuEChERS method was established according to the original QuEChERS cleanup procedure. For the second modified QuEChERS method, the extract was evaporated to dryness and reconstituted in acetonitrile. Subsequently, the analytes in the reconstituted solution were retained by primary secondary amine (PSA) and released from PSA with 1.0% formic acid in methanol. Finally, the eluate was evaporated and dissolved in 0.1% formic acid solution/methanol (v/v, 80:20). All of the samples were analyzed by LC–MS/MS on a Waters Acquity BEH C18 column with 0.1% formic acid in water/methanol as the mobile phase with gradient elution. The matrix effect, recovery, and repeatability, within laboratory reproducibility, and the LODs and LOQs of the two modified QuEChERS sample preparation methods were investigated and compared. Comparative results showed that the second method was obviously superior to the first method.</abstract><cop>England</cop><pub>Elsevier B.V</pub><pmid>24036362</pmid><doi>10.1016/j.jpba.2013.08.026</doi><tpages>7</tpages></addata></record>
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subjects Acetonitriles - chemistry
Amines - analysis
Amines - chemistry
Animal Feed
Baclofen
Baclofen - analysis
Chemistry Techniques, Analytical
Chemistry, Pharmaceutical - methods
Chemistry, Pharmaceutical - standards
Chromatography, Liquid
Cyclohexanecarboxylic Acids - analysis
Excitatory Amino Acid Antagonists - analysis
Feed
Formates - chemistry
GABA-B Receptor Agonists - analysis
Gabapentin
gamma-Aminobutyric Acid - analysis
LC–MS/MS
Mass Spectrometry
Methanol - chemistry
QuEChERS
Reproducibility of Results
Time Factors
Water - chemistry
title Evaluation of two modified quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation methods for the analysis of baclofen and gabapentin in feeds by liquid chromatography tandem mass spectrometry
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