摘要
目的建立腐竹、米线、年糕中乌洛托品的超高压液相色谱-串联质谱分析方法。方法样品经粉碎后,用乙腈提取,MCX小柱净化,Waters ACQUITYTM UPLC BEH HILIC色谱柱分离,最后在电喷雾正离子多反应监测模式下,用超高压液相色谱-串联质谱仪进行分析。结果乌洛托品在1.00～100.00μg/L的范围内呈现良好的线性关系良好,线性方程为Y=2391.11X+253.197,R2大于0.99。该方法检出限(S/N=3)和定量限(S/N=10)分别为0.30μg/kg和1.00μg/kg。在1.00、10.00、50.00μg/kg三个添加水平下,乌洛托品平均回收率为82.0%～107.0%,相对标准偏差为6.3%～15.6%。结论该方法操作简便、检出限低,能够满足腐竹、米线、年糕中乌洛托品检测的要求。
@@@@Objective To establish a method for the determination of urotropine in dried beancurd stick, rice noodleand rice pastry by ultra pressure liquid chrmatography-electrospray tandem mass spectrome-try(UPLC-MS/MS). Methods The samples were ground and extracted by acetonitrile, further purified by MCX solid phase extraction column, and separated by Waters ACQUITYTM UPLC BEH HILIC column. The target compound was detected by UPLC-MS/MS under multiple reaction monitoring (MRM) mode with posi-tive electrospray ionization. Results The method showed a good linearity at the range of 1.00~100.00 μg/L for urotropine with R2>0.99. The limits of detection (LOD) was 0.30 μg/kg and the limits of quantification (LOQ) was 1.00 μg/kg for urotropine. Average recoveries of urotropine varied from 82.0% to 107.0% with rel-ative standard deviations of 6.3%~15.6% at three fortification levels of 1.00, 10.00 μg/kg and 50.00 μg/kg. Conclusion This method has the advantages of simple pretreatment, low detection limit and it is suitable for the determination of urotropine in dried beancurd stick, rice flour and rice pastry.
出处
《食品安全质量检测学报》
CAS
2013年第2期472-478,共7页
Journal of Food Safety and Quality
关键词
腐竹、米线、年糕
超高压液相色谱一质谱/质谱
正离子模式
dried beancurd stick,rice flour,rice pastry
ultra pressure liquid chromatography-electrospraytandem mass spectrometry(UPLC-MS/MS)
positive mode
