建立了枸杞籽油中14种真菌毒素的超高效液相色谱-串联质谱(UPLC-MS/MS)的检测方法,样品以QuEChERS(Quick,Easy,Cheap,Effective,Rugged,Safe)法为前处理技术,优化净化吸附剂组合和用量,改进净化方式,以甲醇-2mmol/L甲酸铵为流动相梯度洗脱,经BEH C18色谱柱(2.1mm×100mm,1.8μm)分离,在电喷雾电离(ESI)正离子模式下采用多反应监测(MRM)进行测定,基质外标法定量.14种真菌毒素在不同浓度下其峰强度和质量浓度呈良好的线性关系(R＞0.9992),样品添加回收试验的平均回收率介于60-120％之间,相对标准偏差为4.16-25.2％之间(n=6).方法检出限为0.03-1.5μg/kg.该方法简单准确,适用于枸杞籽油中14种真菌毒素的同时检测.%A method for the simultaneous determination of 14 Mycotoxins in lycium oil based on optimized quick, easy, cheap, effective, rugged, and safe (QuEChERS) with an improved cleanup procedure using optimized sorbent mixture by ultra high performance liquid chromatography-tandem mass spectrometry was developed. The separation of the analytes was carried out on an BEH C18column (100 mm×2.1 mm, 1.8μm) using the mobile phases of methanol and 2 mmol/L ammonium formate by gradient elution. The detection was performed in the electrospray ion (ESI) positive mode and multiple reaction monitoring (MRM) mode. The matrix-matched calibrations were used to quantify the concentrations.The results showed that the linear calibration curves are in a good linear relationship between chromatographic peak areas and the concentrations (R＞0.9992). For all the samples, the average spiked recoveries ranged 60％ from 120％, and the relative standard deviations (RSDs, n=6) of the method were between 4.16-25.2％.The method is easy and accurate, and can meet the requirement for the determination of 14 mycotoxins in lycium seed oil.
展开▼
