摘要
目的建立QuEChERS-气相色谱串联三重四极杆质谱法测定铁皮石斛中四聚乙醛的方法,并用于温州地区铁皮石斛中四聚乙醛含量测定。方法新鲜铁皮石斛样品经匀浆机匀样后,称取适量样品加乙腈提取、QuEChERS净化,经DB-5MS毛细管色谱柱分离,采用三重四级杆串联质谱的选择反应监测模式检测,基质标准曲线外标法定量。结果四聚乙醛在0.01μg/ml~1.00μg/ml内线性关系良好,相关系数0.9998,添加低浓度0.01 mg/kg、中等浓度0.10 mg/kg、高浓度1.0 mg/kg 3个不同浓度水平,回收率在81.4%~96.1%,相对标准偏差为0.9%,检出限为0.004 mg/kg。用上述建立的方法检测了86份铁皮石斛样本,其中36份样本检出四聚乙醛,总检出率为41.8%(36/86),含量范围为0.004 mg/kg~0.257 mg/kg。结论该检测方法操作简单、方便,回收率与精密度均符合要求,可用于铁皮石斛中四聚乙醛的检测。
Objective To establish a method for determining tetrameric acetaldehyde in dendrobium officinale by QuEChERS coupled with gas chromatography-tandem mass spectrometry(GC-MS/MS),and apply it to the determination of tetrameric acetaldehyde in dendrobium officinale from Wenzhou area.Methods Fresh dendrobium samples were homogenized by a homogenizer,appropriate amounts of samples were weighed and extracted with acetonitrile,and purified with QuEChERS method,and then separated with DB-5MS column and finally detected by tandem mass spectrometry in MRM mode.The external standard calibration was used for the quantification by the matrix standard curve.Results The method had a good linear range when the concentration of tetrameric acetaldehyde was within 0.01μg/ml-1.00μg/ml,with the correlation coefficient greater than 0.9998.The detection limit was 0.004 mg/kg.The recovery rates at three spiking levels were within 81.4%-96.1%,and the relative standard deviation(RSD)was 0.9%.Among 86 samples,36 samples were detected tetrameric acetaldehyde with the detection rate of 41.8%(36/86).The contents ranged from 0.004 mg/kg to 0.257 mg/kg.Conclusion The QuEChERS coupled with GC-MS/MS method is simple and convenient,the recovery and precision meet the requirements.It can provide a reference method for detecting tetrameric acetaldehyde in dendrobium officinale.
作者
郑三燕
陈珞洛
李小东
胡宁恩
林彩琴
ZHENG San-yan;CHEN Luo-luo;LI Xiao-dong;HU Ning-en;LIN Cai-qin(Wenzhou Municipal Center for Disease Control and Prevention,Wenzhou,Zhejiang 325000,China)
出处
《中国卫生检验杂志》
CAS
2021年第14期1684-1686,1690,共4页
Chinese Journal of Health Laboratory Technology
基金
温州市基础性农业科技项目(N20190021)。
