摘要
建立了搅拌棒吸附萃取进行前处理,气相色谱-质谱/质谱法测定饮料和果酱中7种食品防腐剂的方法。饮料和果酱样品用pH=3的30%NaCl溶液稀释,使用搅拌棒进行吸附萃取,吸附在搅拌棒上的防腐剂在热解析单元进行热解析,在冷进样口进行捕集后通过程序升温进入气相色谱,使用串联质谱的多反应监测(MRM)同时检测饮料和果酱中的7种防腐剂(苯甲酸、山梨酸以及对羟基苯甲酸甲酯、对羟基苯甲酸丙酯、对羟基苯甲酸异丙酯、对羟基苯甲酸异丁酯和对羟基苯甲酸庚酯)。苯甲酸、山梨酸在40～400mg/L浓度范围内,对羟基苯甲酸甲酯、对羟基苯甲酸丙酯、对羟基苯甲酸异丙酯和对羟基苯甲酸异丁酯在4～40mg/L浓度范围内,对羟基苯甲酸正庚酯在0.4～4mg/L浓度范围内,各组分响应峰面积与其相应浓度呈良好相关性,r>0.99。苯甲酸和山梨酸的检出限分别为37和47mg/L,对羟基苯甲酸酯类为0.62～6.67mg/L。方法的回收率为84.0%～125.0%;精确度为3.0%～18.1%。本方法灵敏度高,能够同时快速检测饮料和果酱中7种防腐剂。
A method was developed for the determination of seven preservatives in beverage and jam using stir bar sorptive extraction （SBSE） and gas chromatography-tandem mass spectrometry （GC-MS/MS）. Samples were diluted with 30% NaCl solution （pH=3）,and stir bar was added for sorptive extraction. After extraction,the preservatives were desorbed thermally from stir bar,followed by being trapped in cooled injection system and injected into gas chromatography by programmed temperature vaporization. Preservatives were analyzed by tandem mass spectrometry in multiple reactions monitoring. The linearities of the method were good in the range of 40-400 mg/L for sorbic acid and benzoic acid,4-40 mg/L for p-hydroxybenzoic acid methyl,propyl,isopropyl,isobutyl esters,0.4-4.0 mg/L for p-hydroxybenzoic acid heptyl ester,with correlation coefficient above 0.99. The limits of quantification of benzoic acid and sorbic acid were 37 and 47 mg/L,respectively,and p-hydroxybenzoic acid esters ranged from 0.62-6.67 mg/L. The average recoveries were in the range of 84.0%-125.0%,relative standard deviations （RSDs） were in the range of 3.0%-18.1%. The method was sensitive,and could be applied for rapid determination of seven preservatives in beverage and jam.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2010年第8期1156-1160,共5页
Chinese Journal of Analytical Chemistry
关键词
防腐剂
搅拌棒吸附萃取
气相色谱-质谱/质谱
Preservative
Stir bar sorptive extraction
Gas chromatography-tandem mass spectrometry
