液相色谱法快速测定果蔬汁饮料中五氯硝基苯残留量

Rapid determination of pentachloronitrobenzene residue in fruit-vegetable juice by high-performance liquid chromatography

目的:建立高效液相色谱法快速测定果蔬汁饮料中五氯硝基苯残留量的分析方法。方法:用丙酮-石油醚(1:1,v/v)超声提取果蔬汁饮料中的五氯硝基苯,在Shimpack VP-ODS色谱柱(250mm×4.6mm,5μm)上,以甲醇-水(9:1,v/v)为流动相,紫外检测器210mm波长处检测。结果:采用外标法定量,该方法在0.10～10.0mg/L浓度范围内有良好的线性关系,相关系数R2为0.9999,加标回收率均在90%以上,相对标准偏差不大于1.5%,方法最低检出限为0.004mg/kg。结论:通过实验室间能力验证,证明该方法具有快速、准确、样品前处理简便易行等优点,可满足实验室日常快速检测果蔬汁饮料中五氯硝基苯残留量的需求。

Objective：To establish an analysis method for the rapid determination of pentachloronitrobenzen residue in fruit-vegetable juice by high-performance liquid chromatography with an ultraviolet detector.Method：After the sample was extracted from fruit-vegetable juice with acetone-petroleum ether（1：1,v/v）in ultrasonic bath,a satisfactory separation was achieved on a VP-ODS column（250 mm × 4.6 mm,5μm）using methanol-water（9：1,v/v）as the mobile phase and detection was performed on an ultraviolet detector at 210 nm.Results：A good linear relation was obtained in the range of 0.10 ～ 10.0 mg/L,the correlation coefficient（R2） was 0.9999,the recoveries were more than 90%,the relative standard deviation was below 1.5%,and the minimum detection limit was 0.004 mg/kg.Conclusion：Intralaboratory proficiency tests have proved that this method,characterized by rapidness,accuracy and simple and easy pretreatment of samples,can meet the needs for the rapid determination of pentachloronitrobenzen residue in fruit-vegetable juice in a laboratory.