安徽农学通报
安徽農學通報
안휘농학통보
AUHUI AGRICULTURAL SCIENCE BULLETIN
2015年
17期
23-25
,共3页
王斐%王婷%范智超%吴卫东%马文鹏%白昭
王斐%王婷%範智超%吳衛東%馬文鵬%白昭
왕비%왕정%범지초%오위동%마문붕%백소
羰基化合物%环境空气%2,4-二硝基苯肼%温度/溶剂双梯度%液相色谱
羰基化閤物%環境空氣%2,4-二硝基苯肼%溫度/溶劑雙梯度%液相色譜
탄기화합물%배경공기%2,4-이초기분정%온도/용제쌍제도%액상색보
Carbonyl compounds%Ambient air%2,4-dinitrophenylhydrazine%Temperature/solvent double-gradi-ent%Liquid chromatography
该文建立了环境空气中13种碳数在1~8范围内的羰基化合物(6种脂肪醛、2种芳香醛、3种不饱和醛和2种酮)的温度/溶剂双梯度2,4-二硝基苯肼衍生/高效液相色谱分析方法。通过选择合适的色谱柱,优化柱温,用水和乙腈两元溶剂梯度基线分离了13种羰基化合物的衍生物。利用温度梯度解决了13种羰基化合物中C3组分(丙烯醛、丙酮和丙醛)和C4组分(丁烯醛、甲基丙烯醛、丁酮和正丁醛)难以分离的问题。优化的方法在各自的浓度范围内线性相关系数良好(r≥0.9999);对于50.0L的空气样品检出限在0.04~0.19μg/m3(以羰基化合物计);该方法的相对标准偏差小于3.6%;加标回收率在95%~106%,适用于环境空气中羰基化合物的测定。
該文建立瞭環境空氣中13種碳數在1~8範圍內的羰基化閤物(6種脂肪醛、2種芳香醛、3種不飽和醛和2種酮)的溫度/溶劑雙梯度2,4-二硝基苯肼衍生/高效液相色譜分析方法。通過選擇閤適的色譜柱,優化柱溫,用水和乙腈兩元溶劑梯度基線分離瞭13種羰基化閤物的衍生物。利用溫度梯度解決瞭13種羰基化閤物中C3組分(丙烯醛、丙酮和丙醛)和C4組分(丁烯醛、甲基丙烯醛、丁酮和正丁醛)難以分離的問題。優化的方法在各自的濃度範圍內線性相關繫數良好(r≥0.9999);對于50.0L的空氣樣品檢齣限在0.04~0.19μg/m3(以羰基化閤物計);該方法的相對標準偏差小于3.6%;加標迴收率在95%~106%,適用于環境空氣中羰基化閤物的測定。
해문건립료배경공기중13충탄수재1~8범위내적탄기화합물(6충지방철、2충방향철、3충불포화철화2충동)적온도/용제쌍제도2,4-이초기분정연생/고효액상색보분석방법。통과선택합괄적색보주,우화주온,용수화을정량원용제제도기선분리료13충탄기화합물적연생물。이용온도제도해결료13충탄기화합물중C3조분(병희철、병동화병철)화C4조분(정희철、갑기병희철、정동화정정철)난이분리적문제。우화적방법재각자적농도범위내선성상관계수량호(r≥0.9999);대우50.0L적공기양품검출한재0.04~0.19μg/m3(이탄기화합물계);해방법적상대표준편차소우3.6%;가표회수솔재95%~106%,괄용우배경공기중탄기화합물적측정。
A sensitive method based on derivatization with 2,4-dinitrophenylhydrazine(DNPH)followed by temperature/organic solvent double-gradient high performance liquid chromatography analysis of 13 carbonyl compounds(6 aliphatic,2 aromatic and 3 unsaturated aldehydes and 2 ketones)in ambient air was devel?oped.Chromatographic conditions including chromatographic column,column temperature,and detection wave?length were investigated so that the separation was carried out on gradient elution using two solvents(water and acetonitrile). The problem that the C3 series(acrolein-DNPH,acetone-DNPH and propionaldehyde-DNPH)and C3 series(crotonaldehyde-DNPH,methacrolein-DNPH,2-butanone-DNPH and butyraldehyde-DNPH)in 13 carbonyl compounds were difficlut to separate were solved using temperature gradient.The opti?mized method has been validated when rectilinear relationship was obtained between the concentrations of analytes and peak area,and the correlation coefficients were ≥0.999 9. The limits of detection for air sam?ples of 50.0 L varied between 0.04~0.19μg/m3 expressed as carbonyl.The method relative standard devia?tions(%RSD)of all applied carbonyls were lower than 3.6%,and spiked recoveries were in the range of 95%~106%. The method was applied to monitor the concentration of carbonyl compounds in ambient air.