摘要
目的建立检测水果和蔬菜中五氯硝基苯残留量的气相色谱-质谱联用方法。方法样品采用3种不同前处理法进行提取净化后,采用内标法进行定量。优化样品预处理方法,选择适宜的提取溶剂、最佳的超声和振荡时间,采用选择性离子扫描模式进行质谱检测。结论在0.02~0.10μg/m L添加水平,经正己烷提取和Qu ECh ERS柱净化处理的样品,其五氯硝基苯的平均回收率在68.32%~96.82%之间,相对标准偏差为3.4%~5.9%(n=6)。以信噪比S/N=3计算五氯硝基苯的最低检出限为0.002 mg/kg,方法的定量限为0.0067 mg/kg(S/N=10)。结论优化后的前处理方法结果准确、重现性好,检出限相对较低,满足水果和蔬菜中五氯硝基苯残留量的检测要求。
Objective To optimum the pretreatment method for determination of nitrobenzene residues in fruits and vegetables by gas chromatography-mass spectrometry （GC-MS）. Methods Samples were extracted and purified by 3 kinds of different pretreatment methods, and quantified by internal standard method. The sample pretreatment method was optimized, including appropriate extraction solvent, and the best ultrasonic and oscillation time. Selective ion scanning （SIM） mode was used for mass spectrometry detection. Results At the spiked levels of 0.02-0.10 μg/mL, average recoveries of nitrobenzene were 68.32%-96.82%, and the relative standard deviations were 3.4%-5.9% （n=6）. The lowest limit of detection of nitrobenzene was 0.002 mg/kg （S/N=3） and the limit of quantification was 0.0067 mg/kg （S/N=10）. Conclusions The established method has high accuracy and reproducibility, and the limit of detection is relatively low, which can meet the detection requirements of nitrobenzene residues in fruits and vegetables.
作者
赵丽
师真
张瑞雨
农蕊瑜
董玉英
ZHAO Li;SHI Zhen;ZHANG Rui-Yu;NONG Rui-Yu;DONG Yu-Ying(Kunming City Center for Disease Control and Prevention, Kunming 650228, Chin)
出处
《食品安全质量检测学报》
CAS
2017年第9期3619-3622,共4页
Journal of Food Safety and Quality
关键词
水果
蔬菜
五氯硝基苯
气相色谱-质谱联用
fruits
vegetables
quintozene
gas chromatography-mass spectrometry
