CAJ | 학술논문

建立了高效液相色谱法(HPLC)测定含脂羊毛中的灭蝇胺和环虫腈的方法及HPLC.MS/MS确证方法.样品用80 mL 1%三氯乙酸溶液超声提取,MCX柱净化,Hypersil NH_2色谱柱分离,水-乙腈为流动相梯度洗脱,214 nm检测,HPLC-MS/MS确证.在正离子电喷雾电离(ESI+)模式下,环虫腈[M+H]~+及2个主要的特征离子分别为m/z 191.0,150.0和163.0;灭蝇胺[M+H]~+及2个主要的特征离子分别为m/z 167.0,85.0和125.0.在0.05～5.0 mg/L范围内,灭蝇胺和环虫腈均有良好的线性关系,相关系数均为0.9999.本方法的检出限灭蝇胺为0.02 mg/kg,环虫腈为0.01 mg/g.方法的平均加标回收率:灭蝇胺为95.0%～99.9%.环虫腈为83.6%～92.2%.
건립료고효액상색보법(HPLC)측정함지양모중적멸승알화배충정적방법급HPLC.MS/MS학증방법.양품용80 mL 1%삼록을산용액초성제취,MCX주정화,Hypersil NH_2색보주분리,수-을정위류동상제도세탈,214 nm검측,HPLC-MS/MS학증.재정리자전분무전리(ESI+)모식하,배충정[M+H]~+급2개주요적특정리자분별위m/z 191.0,150.0화163.0;멸승알[M+H]~+급2개주요적특정리자분별위m/z 167.0,85.0화125.0.재0.05～5.0 mg/L범위내,멸승알화배충정균유량호적선성관계,상관계수균위0.9999.본방법적검출한멸승알위0.02 mg/kg,배충정위0.01 mg/g.방법적평균가표회수솔:멸승알위95.0%～99.9%.배충정위83.6%～92.2%.
A method for the determination of cyromazine and dicyclanil residues on greasy wool was developed with HPLC and confirmed with HPLC-MS/MS.The cyromazine and dicyclanil residues on greasy wool were extracted with 1% trichloroacetic acid solution with ultrasonic, and cleaned up by MCX SPE column.The HPLC separation was performed on a Hypersil NH_2 using water-acetonitrile (V/V) as the mobile phase with gradient elution and detected at the wavelength of 214 nm.The corroboration method of HPLC-MS/MS was used with electro-spray ionization of positive ion mode.The [ M + H ]~+ and characteristic ions of dicyclanil were m/z 191.0, 150.0 and 163.0, and cyromazine were m/z 167.0, 85.0 and 125.0.The linear ranges of cyromazine and dicyclanil were 0.05-5.0 mg/L.There were good linear relationships between the peak area and concentration in the linear range.The correlation coefficient was 0.9999.The detection limit of cyroma zine was 0.02 mg/kg, and dicyclanil was 0.01 mg/kg.The average recoveries of cyromazine and the dicycla nil were 95.0%-99.9% and 83.6%-92.2%, respectively.