摘要
针对水果蔬菜中乙烯利的残留,建立了三甲基硅重氮甲烷衍生化-气相色谱的分析方法。样品用V（甲醇）：V（盐酸）=9：1的溶液提取,无水乙醚萃取,三甲基硅重氮甲烷衍生化15 min,采用气相色谱-质谱法定性,气相色谱仪-火焰光度检测器（GC-FPD）检测,外标法定量。结果显示：在0.01～2 mg/L范围内,乙烯利的质量浓度与其对应的峰面积间线性关系良好,相关系数大于0.999 6;此方法检出限为0.01 mg/kg,定量限为0.03 mg/kg;在辣椒、番茄、香蕉、苹果和梨的空白果蔬样品中分别添加0.01、0.1和1 mg/kg 3个水平下,回收率为93%～102%,相对标准偏差为4.2%～7.3%。该方法准确度和灵敏度高,抗干扰能力强,能准确并快速测定出水果、蔬菜中乙烯利的残留量。
An analytical method for the determination of ethephon residue in fruits and vegetables was established by using gas chromatography after derivatization with（trimethylsilyl）diazomethane. The samples were extracted with a mixture of hydrochloric acid and methanol（9 ： 1, V/V）. It was then extracted with anhydrous ether and subjected to derivatization by（trimethylsilyl）diazomethane. The extracts were determined by gas chromatography with the external standard method and qualitative by gas chromatography-mass spectrometry. The calibration curve of ethephon residue was linear in the range of 0.01-2 mg/L with correlation coefficients higher than 0.999 6. The detection limit of this method was 0.01 mg/kg and the limit of quantification was 0.03 mg/kg. In the samples of fruits and vegetables at spiked levels from 0.01 mg/kg to 1 mg/kg, the recovery was 93%-102% with the relative standard deviation from 4.2%-7.3%. The method has the advantages of high accuracy, good sensitivity,and strong anti-interference ability, which can be used for the accurate and rapid determination of ethephon residues in fruits and vegetables.
作者
陈克云
王艳丽
沈祥震
鞠香
胡梅
刘艳明
祝建华
CHEN Keyun, WANG Yanli, SHEN Xiangzhen, JU Xiang, HU Mei, LIU Yanming, ZHU Jianhua(Shandong Institute for Food and Drug Control, Ji ＇nan 250101, Chin)
出处
《农药学学报》
CAS
CSCD
北大核心
2018年第4期495-499,共5页
Chinese Journal of Pesticide Science
关键词
三甲基硅重氮甲烷
衍生化
气相色谱
水果
蔬菜
乙烯利
残留
（trimethylsilyl）diazomethane
derivatization
gas chromatography
fruit
vegetable
ethephon
residue
