高效液相色谱-串联质谱法快速检测银耳中的米酵菌酸
高效液相色谱-串联质谱法快速检测银耳中的米酵菌酸
目的建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)快速检测银耳中的米酵菌酸的方法。方法样品以甲醇提取后, 超声振荡, 离心分层, 上清液用甲醇定容。使用空白基质液配置标准曲线对结果进行校正。在优化后的色谱及质谱条件下, 采用(electron spray ionization, ESI)负离子模式进行电离, 并通过多反应监测(multi-selected reaction monitoring, MRM)模式对目标化合物的定量离子和定性离子进行测定。结果米酵菌酸在0.50~50.00 μg/L范围内线性良好, 相关系数r为0.9996, 3个浓度添加水平的平均回收率范围在80.6%~95.6%之间, 相对标准偏差为4.98%~7.21%。方法检出限(limit of detection, LOD)为5.0 μg/kg, 定量限(limit of quantification, LOQ)为15.0 μg/kg。结论该方法操作简便快速, 回收率高、灵敏度高、精密度好, 适合测定银耳基质中的米酵菌酸。
ObjectiveTo establish a method of rapid determination of bongkrekic acid in Tremella by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). MethodsThe sample was extracted with methanol, then it was ultrasonically shaken and centrifuged, and the supernatant was adjusted to volume with methanol. The results were calibrated by a blank matrix configuration standard curve. Under optimized chromatographic and mass spectrometric conditions, ionization was performed using an electron spray ionization (ESI) negative ion mode, and quantitative and qualitative ions of the target compound were determined by a multi-selected reaction monitoring (MRM) mode. ResultsThe linearity of bongkrekic acid was good in the range of 0.50~50.00 μg/L, and the correlation coefficient r was 0.9996. The average recovery of 3 concentration levels were 80.6%~95.6%, and the relative standard deviation was 4.98%?7.21%. The method of limit of detection (LOD) was 5.0 μg/kg, and the limit of quantification (LOQ) was 15.0 μg/kg. ConclusionThe method is simple and rapid, it has high recovery rate, high sensitivity and good precision, which is suitable for the determination of bongkrekic acid in the Tremella.
标题：高效液相色谱-串联质谱法快速检测银耳中的米酵菌酸
英文标题：Rapid determination of bongkrekic acid in Tremella by high performance liquid chromatography-tandem mass spectrometry
作者：
曾令浩 广州检验检测认证集团有限公司,国家加工食品质量检验中心(广东)
李思颖 广州检验检测认证集团有限公司,国家加工食品质量检验中心(广东)
李文倩 广州检验检测认证集团有限公司,国家加工食品质量检验中心(广东)
李柏衡 广州质量监督检测研究院
岑建斌 广州检验检测认证集团有限公司,国家加工食品质量检验中心(广东)
区硕俊 广州检验检测认证集团有限公司,国家加工食品质量检验中心(广东)
中文关键词:高效液相色谱-串联质谱,银耳,米酵菌酸,外标法,
英文关键词:high performance liquid chromatography-tandem mass spectrometry,Tremella,bongkrekic acid,external standard method,
发表日期：2019-05-27
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