摘要
采用液相色谱仪—二极管阵列检测器-离子阱-飞行时间串联质谱仪(LCMS-DAD-IT-TOF)建立减肥类非法添加药物高分辨质谱数据库。样品经乙腈超声提取,提取液经QuEChERS吸附剂净化,以ZORBAX Eclipse AAA色谱柱(150mm×4.6 mm,4.5μm)分离,乙腈和0.1%乙酸为流动相梯度洗脱。筛查限为0.10~0.75 mg/kg,平均回收率在49.4%~88.1%;相对标准偏差为5.0~14.8%。该方法通过紫外光谱确定非法添加药物特征吸收波长,结合滥用药物高分辨质谱数据库,通过精确质量数的检索匹配对非法添加药物实现快速筛查,并使用保留时间、同位素丰度和多级特征碎片离子进行确证。根据多级碎片离子,推导出裂解途径。具有简便、快速、高效、准确等优点。在缺乏标准品或对照品的情况下,即可得到准确可靠的结论。适用于保健食品中非法添加药物的有效快速筛查。
The high resolution mass speetrometry database of weight- loss illegally added drugs was established base on liquid chromatogra- phy-diode array detector-ion trap-time of flight tandem mass spectrometry （LC-DAD-MS-IT-TOF）. The analytes in samples were extracted with aeetonitrile and the extract was purified with the mixed QuEChERS sor- hents. In the chromatographic analysis, target compounds were separated on a ZORBAX Eclipse AAA column （150 mm × 4.6 mm, 4.5 μm） with the gradient elution using the mobile phases of acetonitrile and water containing 0. 1% acetic acid. The results showed that the screening detection limit （SDL）of the target compounds were ranged from 0.10-0.75 mg/kg. The method validation was carried out at SDL levels, and the recoveries were 49.4 %-88.1%, with the relative standard deviations（RSDs） of 5.0%- 14.8 %. The characteristic absorption wavelength of illegally added drugs was determined by UV spectrum. The screening of analytes was performed by precision mass matching and library searching. The retention time, isotopic abun- dance and multiple-stage ion mass spectral was employed to the con {irmation. Moreover, the ion fragmentation patterns of these drugs can be exploited to predict the chemical formula and the fragmentation pathway. This method is simple, fast, credible and high sensitivity, which can be applied to simultaneous screening and identification of illegally added drugs in health foods.
出处
《食品与机械》
CSCD
北大核心
2017年第11期52-56,共5页
Food and Machinery
基金
国家质检总局科技计划项目(编号:2016IK119)
"十二五"国家科技支撑计划项目(编号:2012BAK08B01)
关键词
保健食品
非法添加药物
筛查
离子阱飞行时间串联质谱
Health foods
illegally added drugs
screening
liquid chromatography-ion trap-time of flight tandem mass spectrometry （ LC-MS-IT-TOF）
