现代农业科技
現代農業科技
현대농업과기
XIANDAIHUA NONGYE
2012年
5期
347-348
,共2页
杨娟%吴星祥%冯敏铃%李盛安%李拥军
楊娟%吳星祥%馮敏鈴%李盛安%李擁軍
양연%오성상%풍민령%리성안%리옹군
固相萃取%高效液相色谱-串联质谱%羊肉%β-兴奋剂%残留
固相萃取%高效液相色譜-串聯質譜%羊肉%β-興奮劑%殘留
고상췌취%고효액상색보-천련질보%양육%β-흥강제%잔류
solid phase extraction%high performance liquid chromatography-tandem mass spectrophy%mutton%β-agonists%residues
利用固相萃取-高效液相色谱-串联质谱技术,建立了羊肉中克伦特罗、莱克多巴胺、沙丁胺醇3种β-兴奋剂的测定方法。样品经乙酸铵缓冲溶液提取后,用MCX固相萃取柱净化,以甲酸-乙腈和甲酸-乙酸铵缓冲溶液为流动相,梯度洗脱,采用HPLC—MS/MS电喷雾正离子(ESI^+)电离,多反应监测(MRM)模式检测,外标法定量。结果表明,3种β-兴奋剂在2-100ng/mL范围内均具有良好的线性关系,相关系数不低于0.9988,加标回收率为91-3%~103.8%,相对标准偏差为2.5%-5.7%。该方法准确、灵敏、高效、环保,适用于羊肉中克伦特罗、莱克多巴胺、沙丁胺醇3种β-兴奋剂的同时测定。
利用固相萃取-高效液相色譜-串聯質譜技術,建立瞭羊肉中剋倫特囉、萊剋多巴胺、沙丁胺醇3種β-興奮劑的測定方法。樣品經乙痠銨緩遲溶液提取後,用MCX固相萃取柱淨化,以甲痠-乙腈和甲痠-乙痠銨緩遲溶液為流動相,梯度洗脫,採用HPLC—MS/MS電噴霧正離子(ESI^+)電離,多反應鑑測(MRM)模式檢測,外標法定量。結果錶明,3種β-興奮劑在2-100ng/mL範圍內均具有良好的線性關繫,相關繫數不低于0.9988,加標迴收率為91-3%~103.8%,相對標準偏差為2.5%-5.7%。該方法準確、靈敏、高效、環保,適用于羊肉中剋倫特囉、萊剋多巴胺、沙丁胺醇3種β-興奮劑的同時測定。
이용고상췌취-고효액상색보-천련질보기술,건립료양육중극륜특라、래극다파알、사정알순3충β-흥강제적측정방법。양품경을산안완충용액제취후,용MCX고상췌취주정화,이갑산-을정화갑산-을산안완충용액위류동상,제도세탈,채용HPLC—MS/MS전분무정리자(ESI^+)전리,다반응감측(MRM)모식검측,외표법정량。결과표명,3충β-흥강제재2-100ng/mL범위내균구유량호적선성관계,상관계수불저우0.9988,가표회수솔위91-3%~103.8%,상대표준편차위2.5%-5.7%。해방법준학、령민、고효、배보,괄용우양육중극륜특라、래극다파알、사정알순3충β-흥강제적동시측정。
A soild phase extraction-high performance liquid chromatography-tandem mass spectrophy (HPLC-MS/MS)was developed for determination of three β-agonists such as clenbuterol, ractomine, salbutemol residues in mutton. The samples were extracted by ammonium acetate buffer, and purified by MCX solid-phase extraction column. Using Formic aeid-acetonitrile and formic acid-ammonium acetate buffer as mobile phase by gradient elution, the analysis of target compounds was carried out by HPLC-MS/MS under positive electrospray ionization (ESI^+) and multiple reaction monitoring (MRM)mode. An external standard was employed for quantitative analysis. The calibration curves were in good linearity between the peak area and the concentration of 2 to 100 ng/mL for three β-agonists with correlation coefficients not less than 0.998 8. The spiked recoveries ranged from 91.3% to 103.8% with relative standard deviations of 2.5% to 5.7%. The proposed method is accurate, sensitive and high-efficient ,and is applicable for simultaneous determination of three β-agonists in mutton.