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目的探讨用液相色谱-串联质谱法检测瓶装乳酸饮料中双酚A的样品前处理及测定方法。方法样品在碱性条件下沉淀蛋白质后,用固相萃取小柱提取,甲醇洗脱。样品经色谱柱(2.1 mm×50 mm,5μm)分离,以纯水-甲醇(40∶60,V/V)为流动相分离。采用电喷雾电离负离子模式(ESI-),多反应监测(MRM),外标法定量分析。结果该方法在2.0~100.0μg/L范围内呈良好线性;仪器检出限0.01 ng;当取样量为10 g,方法检出限为0.001μg/kg;双酚A高、中、低加标浓度(80、50、10μg/L)的平均回收率为100.9%~107.5%,变异系数为6.2%~7.6%。结论该方法适用于塑料瓶装乳酸饮料中双酚A含量的测定,具有灵敏度高、前处理方法简单、可批量检测、检测速度快的特点,可推广检测食品样品中痕量双酚A含量。
Objective To investigate the sample preparation and determination of bisphenol A in bottled lactic acid drink by liquid chromatography-tandem mass spectrometry. Methods Samples were precipitated in alkaline conditions, extracted with solid phase extraction cartridge and eluted with methanol. The sample was separated on a column (2.1 mm × 50 mm, 5 μm) and separated by pure water-methanol (40:60, V / V). Electrospray ionization negative ion mode (ESI-), multiple reaction monitoring (MRM), external standard quantitative analysis. Results The method showed a good linearity in the range of 2.0-100.0 μg / L. The detection limit was 0.01 ng. The detection limit was 0.001 μg / kg when the sample volume was 10 g. The average recoveries of concentration (80, 50, 10 μg / L) ranged from 100.9% to 107.5% with coefficients of variation from 6.2% to 7.6%. Conclusion The method is suitable for the determination of bisphenol A content in plastic bottled lactic acid drinks. It has the characteristics of high sensitivity, simple pretreatment method, batch detection and fast detection speed. It can promote the detection of trace amounts of bisphenol A in food samples.