超高效液相色谱-串联质谱法同时测定中药中29种合成着色剂
Simultaneous determination of 29 synthetic colorants in Chinese herbal pieces by UPLC-MS/MS
分类号:R917
出版年·卷·期(页码):2018,38 (6):1029-1035
DOI:
10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------
目的:建立采用超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定中药材及饮片中29种合成着色剂的方法。方法:中药材以70%乙醇为提取溶剂进行超声提取,离心后取上清液以Acquity TM UPLC BEH C18色谱柱(1.7 μm,2.1 mm×100 mm)进行分离,以0.02 mol·L-1醋酸铵溶液和甲醇为流动相进行梯度洗脱,流速为0.2 mL·min-1。采用电喷雾离子源进行正离子模式监测,选择反应监测模式(SRM)用于定量分析。结果:在相应的浓度范围内,29种色素的质量浓度与峰面积呈良好的线性关系,r ≥ 0.95;检测下限在0.1~0.26 ng之间;平均回收率范围为86.3%~116.3%,方法的相对标准偏差为0.61%~3.76%。结论:该方法分析速度快,灵敏度高,检测的色素种类较为全面,可用于中药材中非法染色的筛查。
-----英文摘要:---------------------------------------------------------------------------------------
Objective: To establish a method for simultaneous determination of 29 kinds of synthetic colorants in Chinese herbal medicine by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).Methods: Chinese herbal medicine was extracted with ultrasonic by 70% ethanol.Supernatant liquid was collected after centrifugation and separated on Waters Acquity TM UPLC BEH C18 chromatographic column (1.7 μm,2.1 mm×100 mm).0.02 mol·L-1 ammonium acetate and methanol were used as mobile phase to elute at 0.2 mL·min-1;Selective-reaction monitoring(SRM)scanning was employed for quatification with switching electrospragion source polarity in positive mode.Results: There was a good linear relationship between the mass concentration of 29 pigments and the peak area in the corresponding concentration range(r ≥ 0.95).The detection limit was between 0.1 and 0.26 ng.The average recovery range was 86.3%-116.3%.The relative standard deviation of the method was 0.61%-3.76%.Conclusion: This analysis method has high efficiency and high sensitivity,and detection of pigment types is more comprehensive.Therefore,it can be used for the screening of illegal dyeing in Chinese herbal medicines.
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