福建分析测试
福建分析測試
복건분석측시
FUJIAN ANALYSIS & TESTING
2014年
2期
48-51
,共4页
杨旺火%吴少明%周鹏%刘飞
楊旺火%吳少明%週鵬%劉飛
양왕화%오소명%주붕%류비
QuEChERS方法%盐霉素%高效液相色谱-电喷雾串联质谱%检测
QuEChERS方法%鹽黴素%高效液相色譜-電噴霧串聯質譜%檢測
QuEChERS방법%염매소%고효액상색보-전분무천련질보%검측
QuEChERS%salinomycin%Electrospray ionization Tandem HPLC-MS/MS%detection
建立了分散固相萃取-超高效色谱-电喷雾串联质谱快速测定鸡肉中盐霉素残留的方法。样品经乙腈提取后,采用QuEChERS方法净化,氮吹转换溶剂后,采用Acquity BEH C18柱进行分离,0.3%甲酸水溶液-甲醇体系为流动相,梯度洗脱,电喷雾质谱正离子多反应监测模式测定,外标法定量。结果表明,在优化的条件下对样品进行分析检测,盐霉素的检出限为0.03μg·kg-1,添加水平为5.5~31.4μg·kg-1时,加标回收率为78.2-97.8%,RSD<2.0%(n=6),在0.630~25.2μg·L-1质量浓度范围内呈良好线性,相关系数R2>0.9989。该方法前处理步骤简单,具有较高灵敏度,可用于大批量样品的快速筛查检测。
建立瞭分散固相萃取-超高效色譜-電噴霧串聯質譜快速測定鷄肉中鹽黴素殘留的方法。樣品經乙腈提取後,採用QuEChERS方法淨化,氮吹轉換溶劑後,採用Acquity BEH C18柱進行分離,0.3%甲痠水溶液-甲醇體繫為流動相,梯度洗脫,電噴霧質譜正離子多反應鑑測模式測定,外標法定量。結果錶明,在優化的條件下對樣品進行分析檢測,鹽黴素的檢齣限為0.03μg·kg-1,添加水平為5.5~31.4μg·kg-1時,加標迴收率為78.2-97.8%,RSD<2.0%(n=6),在0.630~25.2μg·L-1質量濃度範圍內呈良好線性,相關繫數R2>0.9989。該方法前處理步驟簡單,具有較高靈敏度,可用于大批量樣品的快速篩查檢測。
건립료분산고상췌취-초고효색보-전분무천련질보쾌속측정계육중염매소잔류적방법。양품경을정제취후,채용QuEChERS방법정화,담취전환용제후,채용Acquity BEH C18주진행분리,0.3%갑산수용액-갑순체계위류동상,제도세탈,전분무질보정리자다반응감측모식측정,외표법정량。결과표명,재우화적조건하대양품진행분석검측,염매소적검출한위0.03μg·kg-1,첨가수평위5.5~31.4μg·kg-1시,가표회수솔위78.2-97.8%,RSD<2.0%(n=6),재0.630~25.2μg·L-1질량농도범위내정량호선성,상관계수R2>0.9989。해방법전처리보취간단,구유교고령민도,가용우대비량양품적쾌속사사검측。
A method for rapid determination of salinomycin in chicken was developed by ultra high performance liquid chromatography-electrospray ionization tandem mass spectrometry with dispersive solid-phase extraction. The compounds were extracted from chicken tissue with acetonitrile and then cleaned up by dispersive solid phase extraction, after solvent exchanged, the salinomycin was analyzed by LC-MS/MS on an Acquity BEH C18 column with methanol-0.3%FA-H2O solution as mobile phase by gradient elution under positive ion multiple reaction monitoring(MRM)mode. It showed, under optimized conditions the limit of detection for salinomycin was 0.03μg·kg-1, the recoveries between 5.5~31.4μg·kg-1spiked levels ranged from 78.2-97.8%, with RSDs less than 2.0%(n=6). The calibration curves was linear in the ranges of 0.630~25.2 μg·L-1, with a correlation coefficient more than 0.9989. Owe to its simple pretreatment, high sensitivity, this method could be used for rapid screening for detection of large quantities of samples.