超高效液相色谱-大气压化学电离-串联质谱法测定烘焙咖啡中丙烯酰胺
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摘要
建立了烘焙咖啡中丙烯酰胺的超高效液相色谱-大气压化学电离-串联质谱(UHPLC-APCI-MS/MS)分析方法。样品经甲醇提取,HLB固相萃取(SPE)小柱净化,Brownlee validated AQ C18色谱柱分离,采用大气压化学电离(APCI)源,正离子扫描和多反应监测(MRM)模式对丙烯酰胺进行检测,内标法定量。结果表明,丙烯酰胺在0.5～100.0μg/L范围内具有良好的线性关系,相关系数(r~2)为0.999,方法检出限为5.0μg/kg,定量限为10.0μg/kg。在100.0、200.0和1 000.0μg/kg添加水平下,丙烯酰胺的回收率为94.6%～115.0%,相对标准偏差(RSD)值为2.8%～3.6%(n=6)。本方法采用APCI源作为离子化方式,能有效地减少咖啡基质对丙烯酰胺的基质干扰,前处理简单,灵敏度高,适用于咖啡中丙烯酰胺的日常检测。
A method using ultra high performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry(UHPLC-APCI-MS/MS) was developed for the determination of acrylamide in coffee. The coffee samples spiked with ~(13)C_3-acrylamide as the internal standard were extracted with methanol, and cleaned using HLB solid phase extraction(SPE) cartridges. The liquid chromatography separation was performed on a Brownlee validated AQ C18 column with isocratic elution. Methanol and 0.1%(volume percentage) formic acid aqueous solution were used as the mobile phase. Identification of acrylamide was achieved by APCI-MS/MS with multiple reaction monitoring(MRM) in the positive mode. The quantification analysis was performed by the internal standard method. The calibration curve showed good linearity with a correlation coefficient of 0.999 in the range of 0.5-100.0 μg/L. The limit of detection(LOD) was 5.0 μg/kg. The limit of quantification(LOQ) was 10.0 μg/kg. Recovery of acrylamide from coffee sample was evaluated at concentrations of 100.0, 200.0 and 1 000.0 μg/kg. The average recoveries of acrylamide were between 94.6%-115.0% with relative standard derivations(RSDs) in the range of 2.8%-3.6%(n=6). This simple, accurate and sensitive method was proven to be suitable for the determination of acrylamide in coffee.
A method using ultra high performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry(UHPLC-APCI-MS/MS) was developed for the determination of acrylamide in coffee. The coffee samples spiked with ~(13)C_3-acrylamide as the internal standard were extracted with methanol, and cleaned using HLB solid phase extraction(SPE) cartridges. The liquid chromatography separation was performed on a Brownlee validated AQ C18 column with isocratic elution. Methanol and 0.1%(volume percentage) formic acid aqueous solution were used as the mobile phase. Identification of acrylamide was achieved by APCI-MS/MS with multiple reaction monitoring(MRM) in the positive mode. The quantification analysis was performed by the internal standard method. The calibration curve showed good linearity with a correlation coefficient of 0.999 in the range of 0.5-100.0 μg/L. The limit of detection(LOD) was 5.0 μg/kg. The limit of quantification(LOQ) was 10.0 μg/kg. Recovery of acrylamide from coffee sample was evaluated at concentrations of 100.0, 200.0 and 1 000.0 μg/kg. The average recoveries of acrylamide were between 94.6%-115.0% with relative standard derivations(RSDs) in the range of 2.8%-3.6%(n=6). This simple, accurate and sensitive method was proven to be suitable for the determination of acrylamide in coffee.
引文
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