【摘要】 建立了液相色谱-串联质谱(HPLC-MS/MS)同时测定禽肉中利巴韦林和金刚烷胺的检测方法。禽肉样品用1%(体积分数)三氯乙酸水溶液-甲醇(1∶1,体积比)提取,经PCX固相萃取柱和QuEChERS方法净化后,以含5 mmol/L乙酸铵水溶液与甲醇为流动相梯度洗脱,BEH HILIC(2.1 mm×100 mm,1.7μm)色谱柱分离,电喷雾正离子模式电离,多级反应监测(MRM)模式进行检测,内标法定量。结果表明,利巴韦林和金刚烷胺在0.50~200μg/L范围内呈良好线性,相关系数均大于0.997。两种目标分析物的方法检出限(S/N≥3)分别为0.30μg/kg和0.15μg/kg,定量下限(S/N≥10)分别为1.00μg/kg和0.50μg/kg,样品在其1倍、2倍、10倍定量下限3个加标水平下的日内回收率为92.5%~104.7%,相对标准偏差(RSD)为3.4%~7.8%;日间回收率为93.3%~106.0%,RSD为6.0%~10.7%。该方法灵敏、简便、准确,可用于禽肉中利巴韦林和金刚烷胺残留的同时检测。更多还原

【Abstract】 A method was developed for the simultaneous determination and identification of ribavirin and amantadine residues in poultry meat by liquid chromatography- tandem mass spectrometry( HPLC-MS / MS). The samples were purified with solid phase extraction column of PCX and QuEChERS method after extraction with 1% trichloroacetic acid- methanol( 1 ∶ 1),then separated on a BEH HILIC column( 2. 1 mm × 100 mm,1. 7 μm) by gradient elution with mobile phases of 5 mmol / L ammonium acetate- methanol. An internal standard method was used for quantitative analysis. The electrospray was operated in positive mode and a multiple reaction monitoring( MRM) as survey scan.The results showed that the calibration curves were linear in the range of 0. 50- 200 μg / L for two analytes with correlation coefficients( r) more than 0. 997. The limits of detection( LODs,S / N ≥ 3)for ribavirin and amantadine were 0. 30 μg / kg and 0. 15 μg / kg, respectively, and the limits of quantitation( LOQs,S / N ≥ 10) were 1. 00 μg / kg and 0. 50 μg / kg,respectively. On the basis of LOQs,the intra-day average recoveries for two analytes in poultry meat samples at three spiked levels( 1,2,10 times LOQ) ranged from 92. 5% to 104. 7% with relative standard deviations( RSDs) of3. 4%- 7. 8%,while the inter-day average recoveries ranged from 93. 3% to 106. 0% with RSDs of6. 0%- 10. 7%. The method was sensitive, convenient and accurate, and could satisfy the demands for detection of ribavirin and amantadine residues in poulrty meat.更多还原