色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
8期
886-889
,共4页
张群%刘春华%吴南村%吴小芳%黎舒怀
張群%劉春華%吳南村%吳小芳%黎舒懷
장군%류춘화%오남촌%오소방%려서부
气相色谱-串联质谱%炔螨特%戊唑醇%溴螨酯%台湾青枣
氣相色譜-串聯質譜%炔螨特%戊唑醇%溴螨酯%檯灣青棘
기상색보-천련질보%결만특%무서순%추만지%태만청조
gas chromatography-tandem mass spectrometry(GC-MS/MS)%propargite%tebuconazole%bromopropylate%Taiwan green jujubes
建立了台湾青枣( Zizyphus mauritiana Lam)中炔螨特、戊唑醇和溴螨酯同时测定的气相色谱-串联质谱(GC-MS / MS)分析方法。样品用乙腈匀浆提取,盐析,石墨化炭黑/氨基混合型固相萃取柱净化,乙腈/甲苯(3:1, v / v)洗脱,浓缩定容后检测。目标化合物经 SLB-5MS 色谱柱(30 m×0.25 mm×0.25μm)分离,采用三重串联四极杆质谱多反应监测(MRM)模式进行定性定量分析。结果表明,在0.01~0.50 mg / kg 添加水平时,3种农药的回收率为75.8%~103.6%,相对标准偏差为1.7%~9.3%( n =5)。方法的线性范围为0.01~0.50 mg / kg,决定系数(R2)﹥0.99。该方法对炔螨特、戊唑醇和溴螨酯的定量限均为0.01 mg / kg,能满足台湾青枣中炔螨特、戊唑醇和溴螨酯残留检测的要求。
建立瞭檯灣青棘( Zizyphus mauritiana Lam)中炔螨特、戊唑醇和溴螨酯同時測定的氣相色譜-串聯質譜(GC-MS / MS)分析方法。樣品用乙腈勻漿提取,鹽析,石墨化炭黑/氨基混閤型固相萃取柱淨化,乙腈/甲苯(3:1, v / v)洗脫,濃縮定容後檢測。目標化閤物經 SLB-5MS 色譜柱(30 m×0.25 mm×0.25μm)分離,採用三重串聯四極桿質譜多反應鑑測(MRM)模式進行定性定量分析。結果錶明,在0.01~0.50 mg / kg 添加水平時,3種農藥的迴收率為75.8%~103.6%,相對標準偏差為1.7%~9.3%( n =5)。方法的線性範圍為0.01~0.50 mg / kg,決定繫數(R2)﹥0.99。該方法對炔螨特、戊唑醇和溴螨酯的定量限均為0.01 mg / kg,能滿足檯灣青棘中炔螨特、戊唑醇和溴螨酯殘留檢測的要求。
건립료태만청조( Zizyphus mauritiana Lam)중결만특、무서순화추만지동시측정적기상색보-천련질보(GC-MS / MS)분석방법。양품용을정균장제취,염석,석묵화탄흑/안기혼합형고상췌취주정화,을정/갑분(3:1, v / v)세탈,농축정용후검측。목표화합물경 SLB-5MS 색보주(30 m×0.25 mm×0.25μm)분리,채용삼중천련사겁간질보다반응감측(MRM)모식진행정성정량분석。결과표명,재0.01~0.50 mg / kg 첨가수평시,3충농약적회수솔위75.8%~103.6%,상대표준편차위1.7%~9.3%( n =5)。방법적선성범위위0.01~0.50 mg / kg,결정계수(R2)﹥0.99。해방법대결만특、무서순화추만지적정량한균위0.01 mg / kg,능만족태만청조중결만특、무서순화추만지잔류검측적요구。
An analytical method was established for the determination of propargite,tebucon-azole and bromopropylate in Taiwan green jujubes( Zizyphus mauritiana Lam)by gas chro-matography-tandem mass spectrometry(GC-MS / MS). The sample was extracted with acetoni-trile from the Taiwan green jujubes after treated with a homogenizer. The organic phase was then separated from water phase by adding NaCl. The extract was further purified on a carbon /NH 2 cartridge with elution solvents of acetonitrile / toluene(3 :1,v / v). Finally,the target ana-lytes were separated by a capillary gas chromatographic column SLB-5MS( 30 m × 0. 25 mm × 0. 25 μm). A tandem quadrupole mass spectrometer operated in either full scan mode or in MS /MS mode for multiple reaction monitoring(MRM)was used for the qualitative and quantitative analysis of the constituents,respectively. The results showed that the average recoveries of the three pesticides ranged from 75. 8% to 103. 6% with the RSDs of 1. 7% -9. 3% at the spiking lev-els from 0. 01 mg / kg to 0. 50 mg / kg(n = 5). The calibration curves showed good linearity in the range of 0. 01-0. 50 mg / kg,with the determination coefficients over 0. 99(R 2﹥0. 99). The lim-its of quantification(LOQs)were 0. 01 mg / kg for propargite,tebuconazole and bromopropylate in Taiwan green jujubes. The method is available for the determination of propargite,tebucon-azole and bromopropylate pesticide residues in Taiwan green jujubes.