Determination of Five Amanita Peptide Toxins in Serum and Urine by SPE-UPLC-MS/MS
扫码查看
点击上方二维码区域，可以放大扫码查看
原文链接
维普
万方数据
建立了适用于人体血清和尿液样本中5种鹅膏肽类毒素的固相萃取/超高效液相色谱-串联质谱(Solid Phase Extraction-Ultra Performance Liquid Chromatography Tandem Mass Spectrometry,SPE-UPLC-MS/MS)分析方法.血清样品加水稀释提取、尿液样品进行离心,两者经HLB固相萃取净化后,采用XSelect HSS T3(150 mm×3 mm,2.5 μm)进行色谱分离,水和0.01％甲酸-乙腈的流动相组合进行梯度洗脱,三重四极杆串联质谱正离子模式进行检测.结果表明,5种鹅膏肽类毒素在1～100 ng·mL-1线性关系好,相关系数均大于0.997,血清样品方法定量限为1.5 ng·mL-1,在3个加标水平下平均回收率为74.9％～114.2％,相对标准偏差为3.1％～17.1％(n=6);尿液样品方法定量限为1.0 ng·mL-1,在3个加标水平下平均回收率为81.8％～104.5％,相对标准偏差为1.2％～12.5％(n=6).本方法简便高效,适用于快速检测突发应急事件中毒患者的血清和尿液中鹅膏肽类毒素.
A solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry(SPE-UPLC-MS/MS)method was developed for the determination of five amanita peptide toxins in serum and urine samples.The serum samples were diluted and extracted with water,and the urine samples were centrifuged.The two samples were purified by HLB solid phase extraction.The XSelect HSS T3(150 mm×3 mm,2.5 μm)was used for chromatographic separation,with 0.01％formic acid-acetonitrile and water as mobile phase for gradient elution,and tandem mass spectrometry ESI positive ion mode detection.The results showed that five amanita peptide toxins showed a good linear relationship in the range from 1 to 100 ng·mL-1,and the correlation coefficients were all greater than 0.997.The limit of quantitation of the serum sample method was 1.5 ng·mL-1.The average recoveries at three spiked levels were 74.9％to 114.2％,and the relative standard deviations were 3.1％to 17.1％(n=6).The limit of quantitation of the urine samples was 1.0 ng·mL-1.The average recoveries at three spiked levels were 81.8％to 104.5％,and the relative standard deviations were 1.2％to 12.5％(n=6).The method is simple and efficient,and is suitable for the rapid detection of five amanita peptide toxins in serum and urine of patients with acute emergency poisoning.
amanita peptide toxinserumurinesolid phase extractionultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
维普
万方数据
