固相萃取高效液相色谱-质谱法同时检测啤酒中5种痕量防腐剂  

Simultaneous Determination of Five Trace Preservatives in Beer by Solid Phase Extraction/High Performance Liquid Chromatography-Mass Spectrometry

作　　者：李小晶[1] 陈旻实[1,2] 戴金兰 唐熙[1,2] 邹哲祥[1] 吕水源 周雪晖[1] 

机构地区：[1]福建出入境检验检疫局技术中心国家消费品安全检测重点实验室国家林木产品重点实验室,福建福州350002 [2]食品安全检测教育部重点实验室(福州大学),福建福州350007

出　　处：《分析测试学报》2013年第8期973-977,共5页Journal of Instrumental Analysis

基　　金：福建省科技计划重点项目(2011Y0001);质检总局科技计划重点项目(2013IK103)

摘　　要：建立了固相萃取高效液相色谱-质谱联用法(SPE/HPLC-MS)同时检测啤酒中5种痕量防腐剂的方法。样品经水浴加热、C18固相萃取柱净化后,采用母离子监测模式检测,外标法定量。5种目标物在0.1～10.0 mg/L范围内线性关系良好,相关系数均大于0.99,3种不同加标水平的平均回收率为62.2%～125.0%,相对标准偏差为0.14%～3.4%。苯甲酸、山梨酸的检出限分别为0.020 mg/L和0.015 mg/L,定量下限为0.060mg/L和0.050 mg/L;3种尼泊金酯类物质的检出限均为0.010 mg/L,定量下限为0.045 mg/L。该方法的净化效果良好,具有较好的灵敏度、回收率和重现性,适用于市售啤酒中防腐剂的检测。A high performance liquid chromatography -mass spectrometric （HPLC -MS） method was established for the simultaneous determination of five trace preservatives in beer. The sample was heat ed in water bath, cleaned up with a C18 solid phase extraction column, and then analyzed under parent ion monitoring mode. Matrix-matched calibration curve was used to determine the trace contents by ex ternal standard method. The method showed good linearities in the range of 0. 1 - 10. 0 mg/L for five targets, with correlation coegicients more than 0. 99. The recoveries at three spiked concentration lev. els ranged from 62. 2% to 125. 0% , with RSDs of 0. 14% -3.4%. The limits of detection（LODs） for benzoic acid and sorbic acid were 0. 020 mg/L and 0. 015 mg/L, and the limits of quantitation（LOQs） were 0. 060 mg/L and 0. 050 mg/L, respectively. While the LODs of three parabens were all 0. 010 mg/L and the LOQs were all 0. 045 mg/L. With good purifying effect, sensitivity, recovery and re peatability, the developed method is suitable for the determination of preservatives in beer for sales.

关 键 词：啤酒 防腐剂 固相萃取 高效液相色谱-质谱 

分 类 号：O657.63[理学—分析化学] S482.294[理学—化学]