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.pdf

第4卷第2期
食品安全质量检测学报
Vol 4 No. 2
2013年4月
Journal of Food Safety and Quality
Apr.,2013
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
张爱芝,张书芬,王全林”,沈坚
(宁波市产品质量监督检验研究院,宁波315041)
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小柱浄化、 Waters ACQUITY 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。结果鸟洛托品在1.00~100.00gL的范围内呈现
良好的线性关系良好,线性方程为Y=2391.1X1253.197,R2大于0.99。该方法检出限S/A=3)和定量限(SN=10)
分别为0.30ugkg和1.00ugkg。在1.00、10.00、50.00ggkg个添加水平下,鸟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。
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
Determination of urotropine in dried beancurd stick, rice flour and rice
pastry by ultra pressure liquid chrmatography-electrospray tandem
mass spectrometry
ZHANG Ai-zhi, ZHANG Shu-fen, WANG Quan-lin, SHEN Jian
Ningbo cademy o/ Oaalit Saperision d Insec ion, Ningbo 315041, China
ABSTRACT: Objective To cstablish a method for the dctermination of urotropine in dried beancurd stick
rice noodleand rice pastry by ultra pressure liquid chrmatography-electrospray tandem mass spectrome-
try(UP C-MS/MS).Methods The samplcs werc ground and cxtracted by acetonitrile, further purificd by
MCX solid phase extraction column, and separated by Waters A CQUITY"UPI. C BHH HIIIC column. The
larget compound was detected by UPLC-MS/MS under multiple reaction monitoring(MRM)mode with posi-
tive electrospray ionization. Results The method showcd a good incarity at the rangc of 1.00-100.00 H/L
for urotropine with R">0.99. The limits of detection(1.01 )) was 0.30 ug/kg and the limits of quantification
(.OQ )was 1.00 ug/kg for urotropine. Average recoveries of urotropine varied from 82.0% to 107.0% with rel
alive slandard deviations of 6.3%0-15.6% al three fortification levels of 1.00, 10.00 ug/ky and 50.00 Hg/kg
Conclusion This method has the advantages of simplc pretreatment, low detection limit and it is suitable
for the determination of urotropine in dried beancurd stick, rice flour and rice pastry
KEY WORDS: dried beancurd stick, ricc flour, rice pastry; ultra pressure liquid chromatography-clcctrospra
*通讯作者:干全林,教投高工主要研究方向为食品安全检测技术及标准化。上-mai:quanlinwang163.com
Corresponding author: WANG Quan-lin, Professional Senior Enginccr, Ningbo Academy of Product Quality Supervision &Inspcction
No.1588,JiangnanRoad,GaoxinDistrict,Ningbo315041,ChinaE-mail:quanlinwang(163.com