摘要
建立快速、简单、准确测定豆酱中活性成分磷脂酰胆碱(PC)与其降解产物溶血磷脂酰胆碱(LPC)和甘油磷脂酰胆碱(GPC)含量的超高效液相色谱-质谱联用(UPLC-MS)分析方法。将豆酱样品经过预处理后,以乙腈、醋酸铵为流动相,使用Waters ACQUITY UPLC超高效液相色谱仪,经ACQUITY UPLC BEH HILIC色谱柱(2.1×100mm,粒径1.7μm)分离,利用质谱定性定量测定其含量。质谱在电喷雾正离子模式下,对m/z782、m/z520和m/z258进行选择离子监测。该方法下PC、LPC和GPC分别在0.191～1.910μg/mL,0.236～2.360μg/mL和0.016～0.160μg/mL范围内峰面积和浓度呈良好的线性关系,相关系数R2PC=0.9959、R2LPC=0.9986和RG2PC=0.9991;PC、LPC和GPC的最低检测限分别为0.05、0.07、0.005μg/mL,最低定量限分别为0.19、0.24、0.016μg/mL;方法的平均回收率为93.2%～97.8%,相对标准偏差为1.5%～3.5%。此方法准确,灵敏度高,样品处理简单,分析时间短,可快速测定豆酱中PC与其降解产物LPC和GPC含量。
UPLC-MS was established to determine the content of PC, LPC and GPC in soybean paste. After pretreatment,the extract of soybean paste was injected directly into the system of UPLC.The analysis was carried out on ACQUITY UPLC BEH HILIC column（2.1 × 100m,1.7μm） ,using acetonitrile and ammonium acetate as the mobile phase for quantification. PC, LPC and GPC was identified by electrospray ionization mass spectrometry （ESI-MS） ,and electrospray was operated in positive ion mode to generate protonated ions.The ion at m/z782, m/z520 and m/z258 was recorded in the selective ionization recording （SIR）. Good linearity between response （ peak area）and concentration was found over a concentration range of 0.191-1.910μg/mL for PC,0.236-2.360μg/mL for LPC,and 0.016-0.160μg/mL for GPC, the correlation coefficient of the calibration curve was 0.9959 for PC, 0.9986 for LPC,and 0.9991 for GPC.The detection limit was 0.05μg/mL for PC,0.07μg/mL for LPC,and 0.005μg/mL for GPC.The quantification limit was 0.19μg/mL for PC,0.24μg/mL for LPC, and 0.016μg/mL for GPC.The average recovery rates were 93.2%-97.8% ,and the relative standard deviations were 1.5%-3.5%.This method is accurate, sensitive,short,and the sample treatment is simple,which can be used as a rapid determination of PC, LPC and GPC in soybean paste.
出处
《食品工业科技》
CAS
CSCD
北大核心
2011年第1期287-289,共3页
Science and Technology of Food Industry
基金
十一五国家科技支撑计划(2009BADB9B05)
