超高压液相色谱-串联质谱法测定腐竹、米线、年糕中的乌洛托品
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1.00～100.00 μg/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0.30 μg/kg 和1.00 μg/kg。在1.00、10.00、50.00 μg/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 positive 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 relative standard deviations of 6.3%~15.6% at three forti?cation 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.
标题：超高压液相色谱-串联质谱法测定腐竹、米线、年糕中的乌洛托品
英文标题：Determination of urotropine in dried beancurd stick, rice flour and rice pastry by ultra pressure liquid chrmatography-electrospray tandem mass spectrometry
作者：
张爱芝 宁波市产品质量监督检验研究院
张书芬 宁波市产品质量监督检验研究院
王全林 宁波市产品质量监督检验研究院
沈坚 宁波市产品质量监督检验研究院
中文关键词:腐竹、米线、年糕,超高压液相色谱一质谱/质谱,正离子模式,
英文关键词:dried beancurd stick, rice flour, rice pastry,ultra pressure liquid chromatography-elec?trospray tandem mass spectrometry(UPLC-MS/MS),positive mode,
发表日期：2013-01-18
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