摘要
建立了液相色谱-线性离子阱-静电场轨道阱高分辨质谱（LC-LTQ-Orbitrap）快速测定蜂胶中杨树胶指标性成分水杨苷含量的方法,并根据精确的母离子和子离子质荷比进行定性和确证,以判断蜂胶中是否掺杂杨树胶。样品经无水乙醇提取,Waters xselect HSS T3色谱柱（3.0 mm×100 mm,3.5μm）分离,以乙腈-0.1%乙酸溶液为流动相,正离子扫描模式进行高分辨质谱检测,外标法定量。结果表明,该方法的线性范围为0.5-25.0μg/m L,相关系数（r）大于0.99。在25.0,150.0,300.0 mg/kg 3个加标水平下的平均回收率为81.6%-91.0%,相对标准偏差为9.0%-11.6%。
A method of high performance liquid chromatography（ HPLC） combined with LTQ- Orbitrap XL mass spectrometry was developed for the analysis of salicin,a characteristic component of poplar tree gum in propolis. With the exact parent ion and fragment ion,whether the propolis contains poplar tree gum could be confirmed. The samples were extracted with ethyl alcohol. The LC separation was performed on a Waters xselect HSS T3（ 3. 0 mm × 100 mm,3. 5 μm） column with acetonitrile- 0. 1% acetic acid solution as mobile phase. The analyte was detected under positive mode. The calibration curve showed a good linearity within the concentration range of 0. 5- 25. 0μg /m L. The average recoveries of salicin ranged from 81. 6% to 91. 0% at the spiked levels of25. 0,150. 0,300. 0 mg / kg with relative standard deviations（ RSDs） less than 11. 6%. The developed method was simple,sensitive and repeatable,and could be used as a screen and confirmatory approach for the analysis of salicin in propolis.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第3期342-346,共5页
Journal of Instrumental Analysis
基金
国家质量监督检验检疫总局科研项目计划(2013IK156)
关键词
高效液相色谱
线性离子阱-静电场轨道阱
高分辨质谱
蜂胶
杨树胶
水杨苷
high performance liquid chromatography（HPLC）
linear ion trap-orbitrap mass spectrometer（LTQ-orbitrap MS）
high-resolution mass spectrometry（HRMS）
propolis
poplar tree gum
salicin
