摘要
用液相色谱-串联四级杆质谱法检测食品中丙烯酰胺的含量。添加氘标记的内标d3_丙烯酰胺于样品中,经纯水提取,用OasisHLB和BondElutAccucat固相萃取柱净化。ZorbaxXDB-C18色谱柱分离,流动相为MeOH-H2O(体积比1∶99)含0.1%HAc溶液,流速0.19mL/min。电喷雾正离子MRM模式检测:丙烯酰胺m/z72→55,内标m/z75→58。内标法定量,方法定量下限(LOQ,S/N>10)为50ng/g,在质量浓度0.005～100μg/mL范围内,峰面积与浓度成良好线性(r>0.998)。本法快速、准确、检出限低、实用性强。
Acrylamide in foods was determined by liquid chromatography with tandem quadrupole mass specˉtrometry.A sample spiked with deuterium_labeled acrylamide_d 3 (internal standard)was extracted with waˉter,and centrifugated at high speed.An aliquot of the supernatant was filtered through a Maxi_Spin(0.45μm PVDF)filter.The filtrate was purified by SPE with Oasis HLB cartridge and Bond Elut Accucat cartridge.Chromatographic separation was carried out on a Zorbax XDB_C 18 column(2.1×150mm,5μm)with elution of methanol-water(1∶99by volume)containing0.1%acetic acid at a flow rate of0.19mL/min.The mass spectrometer was operated in the positive electrospray ionization mode.Quantition was performed using multiple reaction monitoring of the product ion transitions m/z72→55for acrylamide and m/z75→58for acrylamide_d 3 .Linearity of peak area was obtained over a wide range of concentrations(from0.005to100 μg/mL),and the correlation coefficient was greater than0.998.The method had a limit of quantitation(LOQ,S/N>10)of50ng/g.The method was sensitive,reliable,selective and reproducible.
出处
《分析测试学报》
CAS
CSCD
北大核心
2005年第3期82-85,共4页
Journal of Instrumental Analysis
关键词
液相色谱
串联四级杆质谱
丙烯酰胺
食品
Liquid chromatography
Tandem quadrupole mass spectrometry
Acrylamide
Food
