知识与财富的链接
目的采用超高效液相色谱-四级杆/静电场轨道阱高分辨质谱建立固相萃取法快速分析尿液中毒蕈碱残留的检测方法。方法样品直接经固相萃取柱富集和净化,以HSS T_3色谱柱(2.1 mm×100 mm,1.8μm)为分析柱,含0.1%甲酸的乙腈及含0.1%甲酸和4 mmol/L甲酸铵的水溶液作为流动相A、B进行梯度洗脱分离,外标法定量。采用正离子采集模式对样品进行快速筛查,t MSMS采集模式定量分析。结果毒蕈碱在0.05~5μg/L范围内呈良好的线性关系,回归系数(r)大于0.999,该方法的检出限和定量限分别为0.02和0.05μg/L。以空白尿液样品进行0.05、0.1和0.5μg/L 3个水平的加标回收试验,毒蕈碱的平均回收率范围在73.2%~97.9%之间,RSD为2.5%~10.2%。结论本方法简单、灵敏、准确,适用于尿液中毒蕈碱残留的快速筛查和分析测定,可满足临床中毒分析和法医鉴定的检测需求。
To establish a solid phase extraction (SPE)/high-resolution benchtop Q Exactive mass spectrometry (HRMS) method for rapid analysis of muscarine in human urine.Methods Samples were pre-concentrated and cleaned up directly with SPE. The chromatographic analysis was performed on an HSS T3 column with 0.1% formic acid and 4 mmol/L ammonium formate in water/acetonitrile as the mobile phase with gradient elution, and external standard calibration was used for quantification. Results The linearity was within 0.05-5 μg/L, and the coefficient of determination (r) was not less than 0.999 for muscarine. The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.02 and 0.05 μg/L, respectively. The recoveries of the spiked samples at the levels of 0.05,0.1, and 0.5 μg/L ranged from 73.2% to 97.9%, with the relative standard deviations (RSDs) from 2.5% to 10.2%.Conclusion The proposed method is rapid, simple, sensitive and specific enough for the rapid analysis of muscarine in human urine, which is sufficient to meet the requirements of clinical medicine and forensic toxicology.
