离子交换固相萃取-超高效液相色谱-串联质谱法快速测定腐竹中的乌洛托品.pdf

第5卷第10期
食品安全质量检测学报
Vol 5 No 10
2014年10月
Journal of Food Salcly and Quality
cL..20)14
离子交换固相萃取-超高效液相色谱-串联质谱法
快速测定腐竹中的乌洛托品
高洁,陈达炜,东思源,苗虹;赵云峰
(国家食品安全风险评估中心,卫生部食品安全风险评估重点实验室,北京100021)
摘要:目的建立腐竹中乌洛托品的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。方法样品经乙
腈水(1:1,の溶液超声提取,阳离子交换柱净化后,经 Waters Acquity UPI. C BEH HII, IC(2.1mmx100mm,1.7
m)色谱柱分离,在电喷鍔正离子多反应监测模式下进行测定。结果乌洛托品在0.5-1000g1.范围內线性
关系良好,相关系数(以大于0.999方法检出限和定量限分别为6ugkg和20ugkg。在20、40、100ug/kg3个
空白加标水平下,乌洛托品的加标回收率为100.19%~103.9%,相对标准偏差为4.796-8.9%。结论该方法快速、
简便、准确可靠,适用于腐竹中非法添加的乌洛托品的含量测定
关键词:乌洛托品;腐竹:超高效液相色谱-串联三重四级杆质谱法;离子交换固相萃取法
Rapid determination of urotropine in dried beancurd sticks b
ultra-performance liquid chromatography-tandem mass
spectrometry coupled with ion exchange solid phase extraction
GAO Jic, CHEN Da-wci, DONG Si-yuan, MIAO Hong, ZHAO Yun-fcng
(Key Laboratory of Fond afety Risk dsses ment, Ministry of Health, China National Center for Food Safe
Risk Assessment, Beijing 100021, China)
ABSTRAC T Objective To cstablish a method for the determination of urotropine in dried beancurd sticks by
ultra-performance liquid chromatography-tandem mass spectrometry ([Pl C-MS/MS). Mcthods Samples
were ultrasonically extracted by acetonitrile/water(]: 1, y: 7), and then purified by calion exchange solid phase
cxtraction. The analytes were scparated on a Waters Acquity UPLC BEH HILIC column(2.I mm x 100 mm,
1.7 wm)and detected by positive electrospray ination in multiple reactions monitoring(MRM).Results
Ihe method showed a good linearity over the range of 0.5-100.0 ug/L with relative coefficient not less than
0.999. The limit of detection( OD )and the limit of quantification(LOQ )were 6 ug/ky and 20 ug/kg, respec
tively. The avcragc recoveries of urotropine at the spiking levcls of 20, 40 and 100 ug/kg were in the rang
100. 1%0-10390 with the relative standard deviations in the range of.78% Conclusion Ihe method is
rapid, simple and accurale for the determination of urotropine in dried beancurd sticks
KEY WORDS: urotropine; dried beancurd sticks; ultra-performance liquid chromatography-tandem mass
trometry; ion exchange solid phase extraction
基金项目:国家质量监督检验检疫总局公益性行业科研专项(2012104003)
Fund: upported by the pecial Public Welfare Industry Rcscarch of the State Administration of Quality Supervision, Inspection and Quarantinc
通讯作者:苗虹,研究员,主要研究方向为食品安全理化检测与膳食暴露评估。T-mail: machias[sa.neL.cn
Corresponding author: MIAO Hong, Professor. hina National entre for Food Safcty Risk Asscssnncnt, No.7 Panjiayuan Nanli, Chaoyang
District, Bcijing 100021, China. E-mail: miao(acfsa nct cn