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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。
OBJECTIVE To establish a rapid solid phase extraction method for the detection of muscarinic residues in urine by ultra performance liquid chromatography-quadrupole / electrostatic field orbit-well high resolution mass spectrometry. Methods The samples were directly concentrated and purified by solid phase extraction (SPE). The analytical column was HSS T_3 (2.1 mm × 100 mm, 1.8 μm) with 0.1% formic acid in acetonitrile and 0.1% formic acid and 4 mmol / L ammonium formate Aqueous solution as the mobile phase A, B gradient elution separation, external standard method. Samples were rapidly screened using positive ion acquisition mode and quantified by t MSMS acquisition mode. Results The muscarinic acid showed a good linearity in the range of 0.05-5 μg / L, with a regression coefficient (r) greater than 0.999. The limits of detection and quantification were 0.02 and 0.05 μg / L, respectively. The blank urine samples were spiked at 0.05, 0.1 and 0.5 μg / L spiked levels. The average muscarinic recoveries ranged from 73.2% to 97.9% with RSDs ranging from 2.5% to 10.2%. Conclusion The method is simple, sensitive and accurate and suitable for rapid screening and analysis of muscarinic residues in urine to meet the detection needs of clinical poisoning analysis and forensic identification.