色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
8期
867-873
,共7页
郑玲%吴玉杰%赵永锋%李丽华%马燕娟
鄭玲%吳玉傑%趙永鋒%李麗華%馬燕娟
정령%오옥걸%조영봉%리려화%마연연
QuEChERS%高效液相色谱-串联质谱%β-兴奋剂%饲料
QuEChERS%高效液相色譜-串聯質譜%β-興奮劑%飼料
QuEChERS%고효액상색보-천련질보%β-흥강제%사료
QuEChERS%high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)%β-agonists%feed
建立了饲料中克仑特罗、莱克多巴胺、喷布特罗、妥布特罗等18种β-兴奋剂的 QuEChERS 结合高效液相色谱-串联质谱的检测方法。饲料样品加水分散后经4%( v / v)氨水乙腈提取,加入25 mg 十八烷基硅烷( C 18)和50 mg N-丙基乙二胺(PSA)吸附剂分散固相萃取净化后,以高效液相色谱-串联质谱进行定性和定量分析。采用 Agi-lent Zorbax Eclipse XDB-C 18(50 mm×4.6 mm,1.8μm)分析柱,以甲醇-0.1%(v / v)甲酸水溶液为流动相进行梯度洗脱,串联质谱在多反应监测(MRM)正离子模式下进行检测,基质外标法定量。结果表明,18种待测物在质量浓度为5~200μg / L 范围内线性关系良好,相关系数为0.9912~0.9995;在0.05、0.1、0.5 mg / kg 3个浓度加标水平下,饲料中18种β-兴奋剂的平均回收率为78.4%~107.1%,相对标准偏差(RSD)为3.5%~12.3%,定量限(以信噪比≥10计)均为0.05 mg / kg。该方法准确、灵敏,前处理简单,可作为饲料中克仑特罗等18种β-兴奋剂筛选和确认的检测方法。
建立瞭飼料中剋崙特囉、萊剋多巴胺、噴佈特囉、妥佈特囉等18種β-興奮劑的 QuEChERS 結閤高效液相色譜-串聯質譜的檢測方法。飼料樣品加水分散後經4%( v / v)氨水乙腈提取,加入25 mg 十八烷基硅烷( C 18)和50 mg N-丙基乙二胺(PSA)吸附劑分散固相萃取淨化後,以高效液相色譜-串聯質譜進行定性和定量分析。採用 Agi-lent Zorbax Eclipse XDB-C 18(50 mm×4.6 mm,1.8μm)分析柱,以甲醇-0.1%(v / v)甲痠水溶液為流動相進行梯度洗脫,串聯質譜在多反應鑑測(MRM)正離子模式下進行檢測,基質外標法定量。結果錶明,18種待測物在質量濃度為5~200μg / L 範圍內線性關繫良好,相關繫數為0.9912~0.9995;在0.05、0.1、0.5 mg / kg 3箇濃度加標水平下,飼料中18種β-興奮劑的平均迴收率為78.4%~107.1%,相對標準偏差(RSD)為3.5%~12.3%,定量限(以信譟比≥10計)均為0.05 mg / kg。該方法準確、靈敏,前處理簡單,可作為飼料中剋崙特囉等18種β-興奮劑篩選和確認的檢測方法。
건립료사료중극륜특라、래극다파알、분포특라、타포특라등18충β-흥강제적 QuEChERS 결합고효액상색보-천련질보적검측방법。사료양품가수분산후경4%( v / v)안수을정제취,가입25 mg 십팔완기규완( C 18)화50 mg N-병기을이알(PSA)흡부제분산고상췌취정화후,이고효액상색보-천련질보진행정성화정량분석。채용 Agi-lent Zorbax Eclipse XDB-C 18(50 mm×4.6 mm,1.8μm)분석주,이갑순-0.1%(v / v)갑산수용액위류동상진행제도세탈,천련질보재다반응감측(MRM)정리자모식하진행검측,기질외표법정량。결과표명,18충대측물재질량농도위5~200μg / L 범위내선성관계량호,상관계수위0.9912~0.9995;재0.05、0.1、0.5 mg / kg 3개농도가표수평하,사료중18충β-흥강제적평균회수솔위78.4%~107.1%,상대표준편차(RSD)위3.5%~12.3%,정량한(이신조비≥10계)균위0.05 mg / kg。해방법준학、령민,전처리간단,가작위사료중극륜특라등18충β-흥강제사선화학인적검측방법。
A multi-residue method was developed for the simultaneous determination of 18 β-agonist residues( clenbuterol,ractopamine,penbutolol,tulobuterol,etc ) in feed by using QuEChERS sample preparation and high performance liquid chromatography-tandem mass spec-trometry(HPLC-MS / MS). The feed samples were dispersed by water,then the analytes were extracted with acetonitrile containing 4%(v / v)ammonia and cleaned up by QuEChERS method with 25 mg octadecylsilyl( C 18 )and 50 mg primary secondary amine( PSA)adsorbents. The separation of compounds was carried on an Agilent ZORBAX Eclipse XDB-C 18 column(50 mm× 4. 6 mm,1. 8 μm)by a gradient elution using methanol-0. 1%( v / v)formic acid aqueous solu-tion as mobile phase. The analytes were detected by tandem mass spectrometry under multiple reaction monitoring(MRM)mode with positive electrospray ionization( ESI +)and quantified by the matrix-matched external standard method. The results showed that the calibration curves of the 18 β-agonists were linear in the range of 5 - 200 μg / L with correlation coefficients of 0. 991 2-0. 999 5. The average recoveries of the 18 analytes at three spiked levels of 0. 05,0. 1 and 0. 5 mg / kg ranged from 78. 4% to 107. 1% with the relative standard deviations( RSDs)of 3. 5% -12. 3% . The limit of quantification( LOQ,S / N≥10)was 0. 05 mg / kg for each analyte . The developed method is simple and sensitive,and can be applied as a screen and confirmatory method for the analysis of β-agonists in feed.