食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2015年
5期
1706-1712
,共7页
欧阳少伦%邵琳智%谢敏玲%吴映璇%林峰
歐暘少倫%邵琳智%謝敏玲%吳映璇%林峰
구양소륜%소림지%사민령%오영선%림봉
离子淌度差分质谱%抗病毒药%鸡肉?
離子淌度差分質譜%抗病毒藥%鷄肉?
리자창도차분질보%항병독약%계육?
differential?mobility?spectrometry%antiviral?drugs%chicken?muscle??
目的:将离子淌度差分质谱(DMS)技术应用于鸡肉中金刚烷胺和利巴韦林抗病毒药物的残留量分析。方法样品中的金刚烷胺和利巴韦林采用三氯乙酸提取,经磷酸酯酶酶解, PBA固相萃取小柱净化后,选用亲水相互作用色谱柱以5 mmol/L乙酸铵水溶液(含0.1%甲酸)-乙腈为流动相梯度洗脱, DMS结合ESI正离子模式定性定量分析。结果在0.5~5.0μg/L的浓度范围内线性关系良好,方法定量限为1.0μg/L,标准添加水平在1.0、2.0、10μg/L时,回收率在68.4%~112.8%之间,相对标准偏差(n=6)在7.3%~11.2%之间。结论该技术的应用可以显著提高目标化合物的选择性,有效去除基质中的干扰物质,噪音明显降低。
目的:將離子淌度差分質譜(DMS)技術應用于鷄肉中金剛烷胺和利巴韋林抗病毒藥物的殘留量分析。方法樣品中的金剛烷胺和利巴韋林採用三氯乙痠提取,經燐痠酯酶酶解, PBA固相萃取小柱淨化後,選用親水相互作用色譜柱以5 mmol/L乙痠銨水溶液(含0.1%甲痠)-乙腈為流動相梯度洗脫, DMS結閤ESI正離子模式定性定量分析。結果在0.5~5.0μg/L的濃度範圍內線性關繫良好,方法定量限為1.0μg/L,標準添加水平在1.0、2.0、10μg/L時,迴收率在68.4%~112.8%之間,相對標準偏差(n=6)在7.3%~11.2%之間。結論該技術的應用可以顯著提高目標化閤物的選擇性,有效去除基質中的榦擾物質,譟音明顯降低。
목적:장리자창도차분질보(DMS)기술응용우계육중금강완알화리파위림항병독약물적잔류량분석。방법양품중적금강완알화리파위림채용삼록을산제취,경린산지매매해, PBA고상췌취소주정화후,선용친수상호작용색보주이5 mmol/L을산안수용액(함0.1%갑산)-을정위류동상제도세탈, DMS결합ESI정리자모식정성정량분석。결과재0.5~5.0μg/L적농도범위내선성관계량호,방법정량한위1.0μg/L,표준첨가수평재1.0、2.0、10μg/L시,회수솔재68.4%~112.8%지간,상대표준편차(n=6)재7.3%~11.2%지간。결론해기술적응용가이현저제고목표화합물적선택성,유효거제기질중적간우물질,조음명현강저。
Objective To establish a differential mobility spectrometry method for determination of amantadine and ribavirin residues in chicken muscle. Methods The amantadine and ribavirin in sample were extracted by trichloroacetic and enzyme hydrolyzing with acid phosphatase, then purified with PBA cartridge. The targeted compounds were separated on a HILIC column with the gradient elution of 5 mmol/L ammoniumacetate (0.1% formic acid) and acetonitrile as the mobile phases. Quantitative and qualitative were detected by tandem mass spectrometry in positive electrospray ionization and multiple reaction monitoring (MRM) mode with differential mobility spectrometry (DMS) on. Results The method showed a good linearity in the range of 0.5~5.0 μg/L, and the limits of quantification was 1.0 μg/kg. The recoveries in chicken muscle at the 1.0 , 2.0 and 10 μg/kg spiked levels was in the range of 68.4%~112.8% with the relative standard deviations (RSD) in the range of 7.3%~11.2%. Conclusion This method can significantly improve the selection of target analysts, effectively eliminate the matrix interference and reduce the noise.