精细与专用化学品
精細與專用化學品
정세여전용화학품
FINE AND SPECIALTY CHEMICALS
2012年
9期
35-37
,共3页
氯霉素%水产品%液质联用仪
氯黴素%水產品%液質聯用儀
록매소%수산품%액질련용의
chloramphenicol%fishery products%high performance liquid chromatography-tandem mass spectrometry
本实验优化了液相色谱一串联质谱法测定水产品中氯霉素的检测方法。样品经提取、净化和浓缩后,用1.0mL50%的甲醇水溶液定容,采用液相色谱一三重四级杆串联质谱仪、多反应监测扫描模式(MRM)检测和同位素内标法定量。氯霉素检测的线性范围为0.20~20.0ng/mL,定量限为0.20μg/kg。在加标量为1.00μg/kg时,样品加标回收率平均为88.4%,相对标准偏差(RSD)小于20%,满足水产品中氯霉素残留的检测要求。
本實驗優化瞭液相色譜一串聯質譜法測定水產品中氯黴素的檢測方法。樣品經提取、淨化和濃縮後,用1.0mL50%的甲醇水溶液定容,採用液相色譜一三重四級桿串聯質譜儀、多反應鑑測掃描模式(MRM)檢測和同位素內標法定量。氯黴素檢測的線性範圍為0.20~20.0ng/mL,定量限為0.20μg/kg。在加標量為1.00μg/kg時,樣品加標迴收率平均為88.4%,相對標準偏差(RSD)小于20%,滿足水產品中氯黴素殘留的檢測要求。
본실험우화료액상색보일천련질보법측정수산품중록매소적검측방법。양품경제취、정화화농축후,용1.0mL50%적갑순수용액정용,채용액상색보일삼중사급간천련질보의、다반응감측소묘모식(MRM)검측화동위소내표법정량。록매소검측적선성범위위0.20~20.0ng/mL,정량한위0.20μg/kg。재가표량위1.00μg/kg시,양품가표회수솔평균위88.4%,상대표준편차(RSD)소우20%,만족수산품중록매소잔류적검측요구。
In this paper, a high performance liquid chromatography-tandem mass spectrometry (HPLC MS/ MS) method for determining ehloramphenicol in fishery products was optimized. Samples were subjected to decontamination mogenate, extraction, concentration and constant volume prior to HPLC-MS/MS analysis. The analysis was carried out in the multi-reaction monitoring (MRM) mode and internal standard isotope dilution method used for quantification. Calibration curves for the analyte exhibited good linearity over the concentration range from 0.20 to 20.0 ng/mL and its limits of quantification was 0.20μg/kg. The recovery rate was 88.4% with amounts of standard addition of 1.00μg/kg, and relative standard deviations (RSD) was less than 20%. The method can meet the requirement of detection for ehloramphenicol in fishery products.