Yamazaki Y, Ninomiya T
Institute of Food Hygiene, Japan Food Hygiene Association, Yaizu, Japan.
J AOAC Int. 1996 May-Jun;79(3):787-90.
A simple and reliable method was developed for determination of imazalil residues in whole lemons. Imazalil was extracted from lemon samples with ethyl acetate under basic conditions. The ethyl acetate in the extract was evaporated, and the residue was dissolved in dichloromethane. The solution was applied to a solid-phase extraction (diol-bonded silica) cartridge. Imazalil was eluted with methanol and determined by gas chromatography (GC) with nitrogen-phosphorus detection. Recoveries at 4 fortified levels (0.1, 1.0, 2.0, and 5.0 micrograms/g) ranged from 93.3 to 97.8%, with coefficients of variation ranging from 0.2 to 3.0%. The detection limit was 0.05 microgram/g. Fifteen commercial lemon samples were analyzed for Imazalil residues; 10 were positive. Concentrations of imazalil residues ranged from 0.22 to 4.44 micrograms/g. Imazalil-positive samples were confirmed by GC with mass-selective detection (m/z 173, 215, and 217).
开发了一种简单可靠的方法来测定完整柠檬中抑霉唑的残留量。在碱性条件下，用乙酸乙酯从柠檬样品中提取抑霉唑。提取物中的乙酸乙酯被蒸发，残留物溶解于二氯甲烷中。将该溶液应用于固相萃取（二醇键合硅胶）柱。用甲醇洗脱抑霉唑，并用带氮磷检测的气相色谱法（GC）进行测定。在4个加标水平（0.1、1.0、2.0和5.0微克/克）下的回收率为93.3%至97.8%，变异系数为0.2%至3.0%。检测限为0.05微克/克。对15个市售柠檬样品进行了抑霉唑残留分析；10个呈阳性。抑霉唑残留浓度范围为0.22至4.44微克/克。通过带质量选择检测（m/z 173、215和217）的气相色谱法对抑霉唑阳性样品进行了确证。
