热带农业科学
熱帶農業科學
열대농업과학
CHINESE JOURNAL OF TROPICAL AGRICULTURE
2015年
7期
57-62,68
,共7页
万凯%刘家容%陆莹%杨炜君
萬凱%劉傢容%陸瑩%楊煒君
만개%류가용%륙형%양위군
超快速高效液相色谱法%荧光检测%氨基甲酸酯%农药残留
超快速高效液相色譜法%熒光檢測%氨基甲痠酯%農藥殘留
초쾌속고효액상색보법%형광검측%안기갑산지%농약잔류
ultra fast high performance liquid chromatography (UFLC)%fluorescence detector (FLD)%carbamate pesticides%pesticide residues
研究应用超快速高效液相色谱仪柱后衍生荧光检测器同时测定普通白菜中16种氨基甲酸酯类农药残留。对流动相组成、波长选择、梯度洗脱等条件进行比较研究,建立了样品经乙腈提取, SPE-NH2固相萃取柱净化,液相色谱柱后衍生分离,荧光检测(λex=339 nm,λem=445 nm)测定,外标法定量的检测方法。研究表明:基于液相色谱荧光检测条件,16种农药残留在0.025~1.0 mg/L浓度范围内线性关系良好;检出限0.002~0.010 mg/L;平均加标回收率73.0%~103.0%,相对标准偏差(RSD)1.5%~8.8%。该研究确定的方法具有检测范围广、快速、灵敏、准确、重现性好、易推广等特点。
研究應用超快速高效液相色譜儀柱後衍生熒光檢測器同時測定普通白菜中16種氨基甲痠酯類農藥殘留。對流動相組成、波長選擇、梯度洗脫等條件進行比較研究,建立瞭樣品經乙腈提取, SPE-NH2固相萃取柱淨化,液相色譜柱後衍生分離,熒光檢測(λex=339 nm,λem=445 nm)測定,外標法定量的檢測方法。研究錶明:基于液相色譜熒光檢測條件,16種農藥殘留在0.025~1.0 mg/L濃度範圍內線性關繫良好;檢齣限0.002~0.010 mg/L;平均加標迴收率73.0%~103.0%,相對標準偏差(RSD)1.5%~8.8%。該研究確定的方法具有檢測範圍廣、快速、靈敏、準確、重現性好、易推廣等特點。
연구응용초쾌속고효액상색보의주후연생형광검측기동시측정보통백채중16충안기갑산지류농약잔류。대류동상조성、파장선택、제도세탈등조건진행비교연구,건립료양품경을정제취, SPE-NH2고상췌취주정화,액상색보주후연생분리,형광검측(λex=339 nm,λem=445 nm)측정,외표법정량적검측방법。연구표명:기우액상색보형광검측조건,16충농약잔류재0.025~1.0 mg/L농도범위내선성관계량호;검출한0.002~0.010 mg/L;평균가표회수솔73.0%~103.0%,상대표준편차(RSD)1.5%~8.8%。해연구학정적방법구유검측범위엄、쾌속、령민、준학、중현성호、역추엄등특점。
The study aims to establish a method for simultaneous determination of 16 pesticide residues which are Aldicarb-sulfoxide, Aldicarb-sulfone, oxamyl, Methomyl, Hydroxycarbofuran, toxic metabolite, Aldicarb, Tsumacide, Propoxu, Carbofuran, Carbary, XMC, Isoprocarb, Fenobcarb, Methiocarb, Thiodicarb, Promecarb in cabbage by ultra fast high performance liquid chromatograph column derivative fluorescence detector. Meanwhile, the study also aims to the comparison of the composition of mobile phase, wavelength selection, gradient elution at different levels. Samples were ectracted by acetonitrile and purified by SPE-NH2-dispersive solid phase extraction. The colleted solution was analyzed by UFLC-FLD with post-column derivation and quantified by external standard method. The wavelengths were set at 339 nm and 445 nm. The result indicates that the calibration curves of 16 pesticides showed good linear relationship in the concentration of 0.025~1.0 mg/L with correlation coefficients greater than 0.999. The detection limits ranged from 0.002~0.010 mg/L. The recoveries ranged from 73.0%~103.0% with the relative standard deviation (RSD) range of 1.5%~8.8% . The method is characterized as wide range of detection, rapid, sensitive, accurate, repeatable and ease of deployment.