CAJ | 학술논문

建立了气相色谱-负化学源质谱（ GC-NCI/MS）测定蜂蜜和王浆中4种杀虫剂残留量的方法。蜂蜜样品由乙酸乙酯提取、乙二胺-N-丙基硅烷（PSA）净化，而王浆样品经乙腈-水（1：1，v/v）提取、C18固相萃取柱净化，采用GC-NCI/MS测定，外标法定量。结果表明：在50~500μg/L范围内4种农药的线性良好；所有农药的LOD在0.12~5.0μg/kg之间，LOQ在0.40~16.5μg/kg之间；在10、15、20μg/kg 3个添加水平下，4种农药的平均回收率在78.2％~110.0％之间，且 RSD均小于14％。所有农药的测定均没有出现干扰峰。该方法简单、快速，准确度、精密度和选择性高，抗干扰能力强，可用于蜂蜜和王浆中这4种农药的快速检测。
건립료기상색보-부화학원질보（ GC-NCI/MS）측정봉밀화왕장중4충살충제잔류량적방법。봉밀양품유을산을지제취、을이알-N-병기규완（PSA）정화，이왕장양품경을정-수（1：1，v/v）제취、C18고상췌취주정화，채용GC-NCI/MS측정，외표법정량。결과표명：재50~500μg/L범위내4충농약적선성량호；소유농약적LOD재0.12~5.0μg/kg지간，LOQ재0.40~16.5μg/kg지간；재10、15、20μg/kg 3개첨가수평하，4충농약적평균회수솔재78.2％~110.0％지간，차 RSD균소우14％。소유농약적측정균몰유출현간우봉。해방법간단、쾌속，준학도、정밀도화선택성고，항간우능력강，가용우봉밀화왕장중저4충농약적쾌속검측。
A method was developed for the determination of four insecticide residues in honey and royal jelly by gas chromatography-negative chemical ionization mass spectrometry ( GC-NCI/MS). The honey and royal jelly samples were treated with different preparation methods as the result of the different components. The honey sample was extracted with ethyl acetate and cleaned up with primary second amine,and the royal jelly sample was extracted with acetoni-trile-water(1:1,v/v),and cleaned up with a C18 solid-phase extraction column. Finally,the extracts of the honey and royal jelly were analyzed by GC-NCI/MS in selected ion monitoring ( SIM)mode separately. External standard calibration method was used for quantification. The linearities of calibration curves of the four insecticides were good with the correlation coeffi-cients greater than 0. 99 in the range of 50-500 μg/L. The limits of the detection( LODs)of the four insecticides were in the range of 0. 12-5. 0 μg/kg,and the limits of the quantification ( LOQs)were in the range of 0. 40-16. 5 μg/kg. The recoveries of the four insecticides spiked in honey and royal jelly at three spiked levels(10,15 and 20 μg/kg)were in the range of 78. 2%-110. 0%,and the relative standard deviations( RSDs)were all below 14%. The sensitivity and selectivity of this method were good with no interfering peaks. The proposed method is simple, quick and effective to analyze the four insecticide residues in honey and royal jelly.