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目的建立辣椒干中阿维菌素残留量的高压液相色谱-荧光检测器分析方法。方法样品采用乙腈提取,乙腈饱和的正己烷去脂,石墨化碳固相萃取小柱净化,以三氟乙酸酐(trifluoroacetic anhtdride,TFAA)和N-甲基咪唑(1-methylimidazole,NMIM)的乙腈溶液衍生化,用C18柱分离,在激发波长为365 nm,发射波长470nm的条件下高压液相色谱-荧光法检测。结果方法在10~500 ng/mL的浓度范围内线性关系良好,相关系数为r=0.999,检测限为5μg/kg。3个不同浓度水平上进行了加标回收率在90.3%~103.1%,RSD在2.31%~6.93%。结论该方法简便灵敏,准确快速,可用于辣椒干中阿维菌素残留量的测定。
Objective To establish a method for the determination of avermectin residues in dried chili pepper by high pressure liquid chromatography-fluorescence detector. Methods The samples were extracted with acetonitrile, saturated with n-hexane and degreased with acetonitrile, cleaned up with carbon graphite solid-phase extraction cartridges, and eluted with trifluoroacetic anhtdride (TFAA) and N-methylimidazole The solution was derivatized with a C18 column and detected by HPLC at a wavelength of 365 nm and an emission wavelength of 470 nm. Results The method showed a good linearity in the range of 10 ~ 500 ng / mL with a correlation coefficient of r = 0.999 and a detection limit of 5 μg / kg. The spiked recoveries of three different concentration levels ranged from 90.3% to 103.1% with RSDs ranging from 2.31% to 6.93%. Conclusion The method is simple and sensitive, accurate and rapid, and can be used for the determination of avermectin residues in dried peppers.