摘要
建立高效液相色谱—串联质谱法测定纺织品中芦荟苷、芦荟大黄素和大黄酚含量的方法。样品经甲醇60℃超声波浴提取30 min后,在Agilent Eclipse XDB-C18(2.1 mm×150 mm,3.5 m)色谱柱上分离,以10 mmol/L乙酸铵溶液(pH=5.75)和乙腈为流动相进行梯度洗脱。三重四级杆质谱采用电喷雾离子源负离子模式在多反应监测(MRM)模式下检测被分析物,外标法定量。纺织样品在3个加标水平时,平均回收率为85.5%~99.9%,相对标准偏差(RSDs)为1.76%~5.92%。该方法具有快速、灵敏、准确、可重复的特点,可应用于纺织品中芦荟成分的痕量分析。
An ultra effective liquid chromatography-tandem mass spectrometry ( LC-MS/MS ) method has been developed for determinating the contents of aloin , aloe-emodin and chrysophanol in textiles .The samples were prepared by ultrasonically extracting using methanol at 60 ℃for 30 min.The LC separation was performed on an Agilent XDB-C18 column (2.1 mm ×150 mm, 3.5 m) using 10 mmol/L ammonium acetate as solution (pH=5.75) and acetonitrile as the mobile phase in a gradient elution mode .The analyses were tested by a triple-quadrupole mass spectrometer in the multiple reaction monitoring ( MRM) mode using electrospray source with negative mode , and quantified by external standard method .The average recoveries of analyses in textile samples at the three spiked levels were in the range of 85.5%-99.9%with the relative standard deviations being 1.76%-5.92%.The method was proved to be rapid , sensitive , accurate and reproducible and can be applied to the trace analysis of aloe constituents in textiles.
出处
《产业用纺织品》
2013年第8期45-49,共5页
Technical Textiles
基金
国家质监总局科技计划项目(2010QK093)