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超声萃取-高效液相色谱法同时测定进出口食品中常见6种防腐剂

作  者:
林塬;赵涛;张兆辉
单  位:
番禺出入境检验检疫局
关键词:
RP-HPLC;超声萃取;同时测定;防腐剂;食品
摘  要:
使用超声萃取-反相高效液相色谱(HPLC)技术,建立同时分离和检测食物中苯甲酸、山梨酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯6种防腐剂的方法。水-甲醇(5:95,V/V)作为提取溶剂进行超声萃取,采用Supelco Discovery C18反相色谱柱,流动相为乙腈-乙酸铵缓冲溶液(pH4.4)进行梯度洗脱,在1ml/min的流速和254nm的检测波长下14min内6种防腐剂得到良好分离。6种防腐剂线性范围从5μg/ml到100μg/ml,相关系数(r)为0.9997~1.0000。方法的平均回收率为90.1%~106.3%,精密度和稳定性的RSD分别为0.58%~1.79%、0.15%~1.65%,检出限的范围为0.012~0.43μg/ml。本方法的预处理过程简便、快速,应用于30种进出口食品中防腐剂的分析检测,检测结果灵敏、可靠。
译  名:
Ultrasonic Extraction-High Performance Liquid Chromatography for Simultaneous Determination of 6 Common Preservatives in Imported and Exported Foods
作  者:
LIN Yuan,ZHAO Tao,ZHANG Zhao-hui(Panyu Entry-Exit Inspection and Quarantine Bureau,Guangzhou 511400,China)
关键词:
RP-HPLC;ultrasonic extraction;simultaneous determination;preservative;foods
摘  要:
An ultrasonic extraction-reversed phased HPLC method was developed for the simultaneous separation and determination of 6 common preservatives such as benzoic acid,sorbic acid,methylparaben,ethyl P-hydroxybenzoate,nipasol and butyl P-hydroxybenzoate.Samples were extracted with the mixture of water and methanol(5:95,V/V) in ultrasonic field.The gradient elution was carried out on a Supelco Discovery C18 column,with an initial mobile phase of acetonitrile-acetate buffer(pH 4.4) and at the flow rate of 1.0 ml/min.The detector wavelength was set at 254 nm.Under these conditions,the separation of the 6 components was achieved within 14 min.The linear ranges for the determination 6 preservatives by this method were from 5 to 100 μg/ml with a correlation coefficient(r) of 0.9997-1.000,and the limits of detection were 0.012-0.43 μg/ml.The average recoveries for the 6 preservatives in sample spiked at three levels(10,50 and 100 μg/g) were 90.1%-106.3%(n = 3).The RSDs of precision and stability were 0.58%-1.79%(n = 5) and 0.15%-1.65%,respectively.Finally,this method was applied to analysis of these preservatives in 30 different imported and exported food samples.Altogether,the pre-treatment procedure of the developed method is simple and rapid,and the result is sensitive and accurate.

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