食品研究与开发
食品研究與開髮
식품연구여개발
Food Research and Development
2015年
17期
123-128,193
,共7页
丁葵英%许文娟%孙军%郭礼强%李凯
丁葵英%許文娟%孫軍%郭禮彊%李凱
정규영%허문연%손군%곽례강%리개
静电场轨道阱%高分辨质谱%蔬菜%20种氨基甲酸酯
靜電場軌道阱%高分辨質譜%蔬菜%20種氨基甲痠酯
정전장궤도정%고분변질보%소채%20충안기갑산지
orbitrap%high resolution mass spectrometer%vegetables%20 carbamate pesticides
建立蔬菜中20种氨基甲酸酯类化合物高效液相色谱-静电场轨道阱高分辨质谱分析法.样品经乙腈提取,QuEChERS方法对样品净化后,采用高效液相色谱-静电场轨道阱高分辨质谱法对样品中的目标化合物进行定性分析,外标法定量确证.结果表明:20种氨基甲酸酯类农药在0.005μg/mL~0.1μg/mL范围内线性关系均良好,R2均大于0.99,且所有农药定量限(LOQ)(S/N=10)均低于国际限量要求;在0.01、0.02 mg/kg和0.04 mg/kg的添加水平下,蔬菜中20种氨基甲酸酯类农药的平均回收率介于60%~120%之间,相对标准偏差(RSD)不大于5.0%.该方法较为简单,只需全扫描并提取精确质量数即可进行准确定量,受基质干扰小,能很好的满足我国进出口蔬菜中20种农药限量的严格要求,可以用于蔬菜基质中此20种氨基甲酸酯类农药残留的检测.
建立蔬菜中20種氨基甲痠酯類化閤物高效液相色譜-靜電場軌道阱高分辨質譜分析法.樣品經乙腈提取,QuEChERS方法對樣品淨化後,採用高效液相色譜-靜電場軌道阱高分辨質譜法對樣品中的目標化閤物進行定性分析,外標法定量確證.結果錶明:20種氨基甲痠酯類農藥在0.005μg/mL~0.1μg/mL範圍內線性關繫均良好,R2均大于0.99,且所有農藥定量限(LOQ)(S/N=10)均低于國際限量要求;在0.01、0.02 mg/kg和0.04 mg/kg的添加水平下,蔬菜中20種氨基甲痠酯類農藥的平均迴收率介于60%~120%之間,相對標準偏差(RSD)不大于5.0%.該方法較為簡單,隻需全掃描併提取精確質量數即可進行準確定量,受基質榦擾小,能很好的滿足我國進齣口蔬菜中20種農藥限量的嚴格要求,可以用于蔬菜基質中此20種氨基甲痠酯類農藥殘留的檢測.
건립소채중20충안기갑산지류화합물고효액상색보-정전장궤도정고분변질보분석법.양품경을정제취,QuEChERS방법대양품정화후,채용고효액상색보-정전장궤도정고분변질보법대양품중적목표화합물진행정성분석,외표법정량학증.결과표명:20충안기갑산지류농약재0.005μg/mL~0.1μg/mL범위내선성관계균량호,R2균대우0.99,차소유농약정량한(LOQ)(S/N=10)균저우국제한량요구;재0.01、0.02 mg/kg화0.04 mg/kg적첨가수평하,소채중20충안기갑산지류농약적평균회수솔개우60%~120%지간,상대표준편차(RSD)불대우5.0%.해방법교위간단,지수전소묘병제취정학질량수즉가진행준학정량,수기질간우소,능흔호적만족아국진출구소채중20충농약한량적엄격요구,가이용우소채기질중차20충안기갑산지류농약잔류적검측.
A method with the High Resolution Benchtop Oritrap Mass Spectrometer was established to rapid screen and identify accurate Mass of 20 carbamate pesticides in vegetables.The samples were extracted by acetonitrile and purified by the QuEChERS,then qualitatively analyzed with the LC-OBMS and quantitatively analyzed with the external standard method.The results indicated the linearity of the method was good between 0.005μg/mL and 0.1μg/mL,and all the limits of quantities (LOQ) of this method can meet the international standard.Meanwhile,the average percent recoveries of the twenty pesticides ranged from 60%to 120%,and the relative standard deviations (RSDS) were all less than 5.0%,at three different addition levels (0.01,0.02 and 0.04μg/mL).This simple method,which can exactly quantitative analyze just by full scaning and extracting exact mass number,and can overcome the matrix-effect influence,can be used for the detection of the 20 carbamate pesticides in vegetables,perfectly satisfying the pesticide residues limit requirements.