福建分析测试
福建分析測試
복건분석측시
FUJIAN ANALYSIS & TESTING
2012年
3期
6-11
,共6页
固相萃取%育苗水%超高效液相色谱-串联质谱法%矮壮素和助状素残留%消解动态
固相萃取%育苗水%超高效液相色譜-串聯質譜法%矮壯素和助狀素殘留%消解動態
고상췌취%육묘수%초고효액상색보-천련질보법%왜장소화조상소잔류%소해동태
SPE%Seeding water%UPLC-MS/MS%ASE%Chlormequat and mepiquat residues%dissipation trend
建立了育苗水中矮壮素和助状素的固相萃取-超高效液相色谱-串联质谱法（SPE-UPLC-MS/MS）测定方法。样品直接采用弱阳离子固相萃取柱净化;在粒径5μm的亲水作用色谱柱上用SeQuant ZLC-HILIC MEKCK色谱柱进行分离;电喷雾正离子（ESI＋）模式电离,多反应监测（MRM）模式检测。以保留时间和特征离子定性、外标法定量。结果表明矮壮素和助状素在0.2~10 ng/mL的空白添加浓度范围内线性良好（r2〉0.999）,在2.0、5.0、10ng/mL的添加水平范围内,平均回收率分别为89.1.0%~107.1%和102.3%~105.4%,相对标准偏差（RSD）分别为8.5%~29.5%和5.5%~23.0%,矮壮素和助壮素的检出限（LOD）为0.005ng/mL,测定低限（LOQ）为0.02ng/mL,水体中矮壮素和助状素的消解动态研究结果表明,矮壮素和助状素在水体中消解速度缓慢,施药42天后才能减少到96%以上。
建立瞭育苗水中矮壯素和助狀素的固相萃取-超高效液相色譜-串聯質譜法（SPE-UPLC-MS/MS）測定方法。樣品直接採用弱暘離子固相萃取柱淨化;在粒徑5μm的親水作用色譜柱上用SeQuant ZLC-HILIC MEKCK色譜柱進行分離;電噴霧正離子（ESI＋）模式電離,多反應鑑測（MRM）模式檢測。以保留時間和特徵離子定性、外標法定量。結果錶明矮壯素和助狀素在0.2~10 ng/mL的空白添加濃度範圍內線性良好（r2〉0.999）,在2.0、5.0、10ng/mL的添加水平範圍內,平均迴收率分彆為89.1.0%~107.1%和102.3%~105.4%,相對標準偏差（RSD）分彆為8.5%~29.5%和5.5%~23.0%,矮壯素和助壯素的檢齣限（LOD）為0.005ng/mL,測定低限（LOQ）為0.02ng/mL,水體中矮壯素和助狀素的消解動態研究結果錶明,矮壯素和助狀素在水體中消解速度緩慢,施藥42天後纔能減少到96%以上。
건립료육묘수중왜장소화조상소적고상췌취-초고효액상색보-천련질보법（SPE-UPLC-MS/MS）측정방법。양품직접채용약양리자고상췌취주정화;재립경5μm적친수작용색보주상용SeQuant ZLC-HILIC MEKCK색보주진행분리;전분무정리자（ESI＋）모식전리,다반응감측（MRM）모식검측。이보류시간화특정리자정성、외표법정량。결과표명왜장소화조상소재0.2~10 ng/mL적공백첨가농도범위내선성량호（r2〉0.999）,재2.0、5.0、10ng/mL적첨가수평범위내,평균회수솔분별위89.1.0%~107.1%화102.3%~105.4%,상대표준편차（RSD）분별위8.5%~29.5%화5.5%~23.0%,왜장소화조장소적검출한（LOD）위0.005ng/mL,측정저한（LOQ）위0.02ng/mL,수체중왜장소화조상소적소해동태연구결과표명,왜장소화조상소재수체중소해속도완만,시약42천후재능감소도96%이상。
A method for determination of chlormequat and mepiquat in seeding water by accelerated solvent extraction-Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry（ASE-UPLC-MS/MS） was established.The sample was cleaned up by WCX solid phase extraction column;The target compounds were separated on SeQuant ZLC-HILIC MEKCK.The residues of chlormequat and mepiquat were obtained under the electrospray ionization in positive ion mode（ESI＋） and multiple reaction monitoring（MRM） mode;The matrix-matched external standards calibration curves were used for quantitative analysis,retain time and feature ion were used for qualitative determination.The linear range was 0.2~10μg/kg and the correlation coefficients（r2） was no less than 0.9990,The average recoveries of chlomequat and mepiquat from seeding water in the three spiked range of 2.0,5.0 and 10.0μg/kg were in the range of 89.1.0%~107.1% and 102.3%~105.4% respectively with relative standard deviations in the range of 8.5%~29.5% and 5.5%~23.0% respectively.The limits of detection and limits of quantitation for the target compounds were 0.2ng/mL and 0.001ng/mL respectively.With the established method,the dissipation rate of chlormequat and mepiquat in water was studied,showing that the target compounds will decrease to 96% or more at about 42days.
