Determination of Vanillin and Ethyl-Vanillin in Milk Powder by Headspace Solid-Phase Microextraction Coupled with Gas Ch
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Determination of Vanillin and Ethyl-Vanillin in Milk Powder by Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry Zhiyuan Wang 1,2 & Guangfeng Zeng 1,2 & Xiaoqun Wei 1,2 & Bo Ding 1,2 & Cheng Huang 3 & Baojun Xu 4
Received: 5 November 2015 / Accepted: 29 April 2016 # Springer Science+Business Media New York 2016
Abstract A method for determination of vanillin and ethylvanillin in milk powder by auto headspace solid-phase microextraction (SPME) coupled with gas chromatographymass spectrometry (GC-MS) was established. Vanillins in sample were extracted with SPME through a fused-silica fiber coated with divinylbenzene/polydimethylsiloxane. The analytes were desorbed by GC at 260 °C for 5 min and separated on a DB-5MS capillary column and detected by MS with EI source by selected ion monitoring mode (EI-SIM). As a result, the limit of detection of vanillin and ethyl-vanillin was 0.1 and 0.05 mg/kg. The spiked recovery was between 90.0 and 100 %, and the RSD ranged from 1.9 to 5.1 % (n = 6). This method eliminated the interferences from complicated matrix effectively. The method was successfully applied for quick determination of vanillin and ethyl-vanillin content in milk powder samples. Keywords Headspace . Solid-phase microextraction . GC-MS . Vanillin . Ethyl-vanillin . Milk powder * Xiaoqun Wei [email protected] * Baojun Xu [email protected] 1
Guangdong Inspection and Quarantine Technology Center, Guangzhou 510623, China
2
Guangdong Key Laboratory of Import and Export Technical Measures of Animal, Plant and Food, 66, Huacheng Road, Zhujiang Newtown, Guangzhou, Guangdong Province 510623, China
3
Jinan University, Guangzhou, China
4
Food Science and Technology Program, Beijing Normal University-Hong Kong Baptist University United International College, 28, Jinfeng Road, Tangjiawan, Zhuhai, Guangdong Province 519085, China
Introduction Vanillins, including vanillin (3-methoxyl-4-hydroxy benzaldehyde) and ethyl-vanillin (3-ethoxyl-4-hydroxy benzaldehyde), are important flavoring additives in food industry. Vanillin and ethyl-vanillin are widely used as food flavor enhancers due to their vanilla aroma and strong milky flavor. So far, there is no national standard method for vanillin determination. GB2760-2014 claims that no flavoring agent should be added in infant formula food for infants within 0–6 months old. In formula food for infants over 6 months old and children, the maximum usage of vanillin, ethyl-vanillin, and vanilla extract are 5 mg/100 mL (volume of ready-to-use) instant food and the defined amount according to processing need, respectively. Vanillin is allowed to be used in infant supplementary cereal food, and the maximum usage is 7 mg/100 g instant food (GB/T 2760-2014). In July 2012, it was reported that nationally forbidden amount of vanillin was detected in several foreign brand phase milk powder. Therefore, it is obvious that a quick and effective analysis method is needed for determining the vanillin content in food. Solid-phase microextraction (SPME) is
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