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

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.