加速溶剂萃取-超高效液相色谱-串联质谱快速测定棉花中残留的8种脱叶.pdf

加速溶剂萃取-超高效液相色谱-串联质谱快速测定棉花中残留

的8种脱叶剂

吴刚;董锁拽;潘璐璐;赵珊红;王力君;郭方龙;李丹

【摘要】采用加速溶剂萃取结合超高效液相色谱-串联质谱(UPLC-MS/MS)技术,

建立了一种快速提取和测定棉花中8种脱叶剂(噻苯隆、脱叶磷、甲基苯噻隆、脱

落酸、氟酮唑草酯、敌草隆、百草枯、嘧草硫醚)的分析方法.样品经提取、浓缩,乙

腈-水溶液(1∶9,v/v)溶解,采用AcquityUPLC(R)HSST3柱(50mm×2.1

mm,1.8μm)分离,以乙腈-0.05％(v/v)甲酸水溶液为流动相,梯度洗脱,电喷雾正离

子模式多反应监测,外标法定量.该方法在0.01～0.3mg/L范围内线性关系良好(r＞

0.99),在添加含量水平为0.l、0.5、1.0mg/kg时,平均回收率范围为

(84.18±8.04)％～(95.99±6.76)％,相对标准偏差(RSD)为7.04％～10.60％,方法

检出限(LOD)为0.8～29μg/kg,方法定量限(LOQ)为2.5～96μg/kg.该方法操作

简便、快捷、灵敏、准确,适合棉花中8种脱叶剂的确证和定量测定.%Anovel

methodhasbeendevelopedfortherapidextractionanddeterminationof

eightdefoliantsincluding

thidiazuron,butiphos,methabenzthiazuron,abscisicacid,carfentrazone-

ethyl,diuron,paraquat,andpyrithiobac-sodiumincottonbyaccelerated

solventextraction(ASE)coupledwithultraperformanceliquid

chromatography-tandemmassspectrometry(UPLC-MS/MS).Thedefoliants

incottonwereextractedbyASEandtheextractsweredriedbya

rotavapor,thenredissolvedinthesolventsofacetonitrileandwater(1∶

9,v/v).ThechromatographicanalysiswasperformedonanAcquityUPLC

（R）HSST3column(50mm×2.1mm,1.8μm)byagradientelution

employingofacetonitrileand0.05％(v/v)formicacidasmobile

phases.Theanalytesweredetectedbyelectrosprayionization(ESI)tandem

massspectrometrywithmultiplereactionmonitoring(MRM)inpositive

ionmode.Goodlinearities(r＞0.99)wereobservedbetween0.01and0.3

mg/Lforallthecompounds.Therecoveriesandrelativestandard

deviations(RSDs)wereobtainedbyspikinguntreatedsampleswiththe

eightdefoliantsat0.1,0.5and1.0mg/kg.Theaveragerecoveriesofthe

eightdefoliantswerefrom(84.18±8.04)％to(95.99±6.76)％.The

precisionvaluesexpressedasRSDswerefrom7.04％to10.60％(n=6).The

limitsofdetectionwere0.8-29μg/kgandthelimitsofquantificationwere

2.5-96μg/kgfortheanaly