QuEChERS/超高效液相色谱-串联质谱法同时测定大米中16种香豆素和香兰素及其衍生物

Simultaneous Determination of 16 Coumarins and Vanillins and Their Derivatives in Rice by QuEChERS/Ultra-high Performance Liq⁃uid Chromatography-Tandem Mass Spectrometry

建立了大米中16种香豆素和香兰素及其衍生物的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。大米样品采用1%甲酸乙腈提取,150 mg C_(18)与450 mg无水MgSO_(4)吸附剂净化,采用Agilent SB-C_(18)色谱柱(2.1 mm×50 mm,1.8μm)分离,0.2%甲酸水溶液(含5 mmol/L甲酸铵)和乙腈为流动相梯度洗脱,在电喷雾离子源正负离子模式下采用多反应监测模式(MRM)进行测定,以基质匹配标准溶液内标法定量。结果显示,16种待测组分在各自质量浓度范围内线性关系良好(r≥0.998),方法检出限为0.001~0.400 mg/kg,定量下限为0.004~0.600 mg/kg,平均回收率为71.3%~120%,相对标准偏差(RSD,n=6)为1.6%~6.5%,日内RSD(n=6)为1.0%~8.8%,日间RSD(n=3)为0.60%~14%。该法前处理简单易操作、灵敏度高、准确性好,适用于大米中香豆素与香兰素及其衍生物的同时检测。

A ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the determination of 16 coumarins and vanillins and their derivatives in rice.The rice sample was extracted by acetonitrile with 1%formic acid,purified with a combined dadsorbent with 150 mg C_(18) and 450 mg anhydrous MgSO_(4).The chromatography separation for the analytes was achieved on an Agilent SB-C_(18) column(2.1 mm×50 mm,1.8μm),and gradient elution was performed using 0.2%formic acid solution(containing 5 mmol/L ammonium formate)and acetonitrile.The analytes were determined by multiple reaction monitoring(MRM)of electrospray ionization in positive and negative ion modes,and quantified by matrix-matched internal standard method.The 16 components measured had good linear relationships within their respective mass concentration ranges(r≥0.998).The limits of detection were 0.001-0.400 mg/kg,and the limits of quantitation were 0.004-0.600 mg/kg.Average recoveries of the 16 components ranged from 71.3%to 120%,the relative standard deviations(RSDs,n=6)ranged from 1.6%to 6.5%,the intra-day RSDs(n=6)ranged from 1.0%to 8.8%,and the inter-day RSDs(n=3)ranged from 0.60%to 14%.The method is simple and easy to operate,with high sensitivity and accuracy,and is suitable for the simultaneous determination of coumarins and vanillins and their derivatives in rice.