摘要
采用MCX固相萃取柱净化,以超高效液相色谱-串联质谱(UPLC-MS/MS)法建立了香辛调料中曲托喹酚的测定方法。样品采用0.2%酸性乙醇提取,经MCX柱净化浓缩后,在ACQUITY BEH C18色谱柱上以乙腈和0.1%甲酸水溶液为流动相梯度洗脱,UPLC-MS/MS以MRM方式进行定量分析。结果表明,曲托喹酚在0.1~50 ng/mL范围内线性关系良好,相关系数(r)大于0.998,方法的检出限(LOD)为0.2μg/kg,定量下限(LOQ)为0.5μg/kg。化合物在不同基质的4个加标水平(0.5、2、10、100μg/kg)下的回收率为74.5%~98.8%,相对标准偏差(RSD)为3.1%~9.1%。该方法灵敏、准确、可靠,可用于香辛调料中曲托喹酚的测定。
An ultra-performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS)method was developed for the determination of tretoquinol in pungent spice with MCX solidphase extraction(SPE)purification.The samples were extracted with 0.2%acid ethanol,purified with a MCX column,and quantified by UPLC-MS/MS in MRM mode after gradient elution on an ACQUITY BEH C18 column with acetonitrile and 0.1%formic acid solution as mobile phase.The results showed that the calibration curves were linear in the range of 0.1-50 ng/mL with correlation coefficients(r)more than 0.998.The limits of detection(LODs)were 0.2μg/kg and the limits of quantitation(LOQs)were 0.5μg/kg.The average recoveries of tretoquinol at four different spiked levels(0.5,2,10,100μg/kg)ranged from 74.5%to 98.8%,with relative standard deviations(RSD)of 3.1%-9.1%.The proposed method is sensitive,accurate and reliable,and could be used for the determination of tretoquinol in pungent spice.
作者
张海超
王敬
贾海涛
李玮
艾连峰
康维钧
ZHANG Hai-chao;WANG Jing;JIA Hai-tao;LI Wei;AI Lian-feng;KANG Wei-jun(Shijiazhuang Customs Technology Center,Shijiazhuang 050051,China;School of Public Health,Hebei Medical University,Shijiazhuang 050017,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2021年第7期1086-1090,共5页
Journal of Instrumental Analysis
基金
总署科技计划项目(2019HK112)
河北省科技计划项目(19226614D)
河北省科技计划项目(19225503D)。
