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时间:2018-04-16
《高效液相色谱_串联质谱法测定牛_羊_奶中阿莫西林的残留》由会员上传分享,免费在线阅读,更多相关内容在学术论文-天天文库。
1、华南农业大学学报2014,35(4):16-21http:∥xuebao.scau.edu.cnJournalofSouthChinaAgriculturalUniversitydoi:10.7671/j.issn.1001-411X.2014.04.004李帅鹏,黄显会,许颖,等.高效液相色谱-串联质谱法测定牛(羊)奶中阿莫西林的残留[J].华南农业大学学报,2014,35(4):16-21.高效液相色谱-串联质谱法测定牛(羊)奶中阿莫西林的残留李帅鹏,黄显会,许颖,郭春娜,孔祥凯(华南农业大学,国家兽药残留基准实验室,广东广
2、州510642)摘要:【目的】建立奶中阿莫西林残留检测的高效液相色谱-串联质谱方法.【方法】2g样品经乙醇沉淀蛋白质后,转入梨形瓶中旋转蒸发浓缩至约0.5mL左右,用pH4.5乙酸铵溶液定容,净化后检测.流动相为乙腈和体积分数0.1%甲酸水溶液,梯度洗脱,经Luna5μmC18色谱柱分离,采用电喷雾电离,多反应监测正离子模式对阿莫西林进行定量分析.【结果和结论】采用基质匹配法对奶中阿莫西林的含量进行标准校正,在阿莫西林质量浓度为1~400-1μg·L范围内呈现良好的线性关系,相关系数>0.999;奶中加标样品的检出限(按信噪比S
3、/N≥3计)为1-1-1-1μg·kg,定量限(按信噪比S/N≥10计)为2μg·kg.在定量限、1/2最高残留限量(5μg·kg)、最高残留限-1-1量(10μg·kg)、2倍最高残留限量(20μg·kg)添加水平下,奶中阿莫西林的平均回收率为75.6%~91.0%,相对标准偏差为1.6%~10.2%.关键词:高效液相色谱-串联质谱;阿莫西林;奶;残留检测中图分类号:O657.63文献标志码:A文章编号:1001-411X(2014)04-0016-06Determinationofamoxicillinresiduesinm
4、ilkbyhighperformanceliquidchromatography-tandemmassspectrometryLIShuaipeng,HUANGXianhui,XUYing,GUOChunna,KONGXiangkai(NationalReferenceLaboratoryofVeterinaryDrugResidues(SCAU),SouthChinaAgriculturalUniversity,Guangzhou510642,China)Abstract:【Objective】Ananalyticalmeth
5、odwasdevelopedforthedeterminationofamoxicillinresiduesinmilkbyhighperformanceliquidchromatography-tandemmassspectrometry(HPLC-MS/MS).【Meth-od】Atwo-grammilksamplewasdeproteinizedbyethanol.Thesupernatantwastransferredintoapear-shapedbottletobeevaporatedtoabout0.5mL,and
6、theresiduewasdissolvedwithammoniumacetateso-lution.ThesamplewasdeterminedbyHPLC-MS/MSafterthepurification.Thechromatographicsepara-tionwasachievedonaLuna5μmC18columnusing0.1%formicacidinwaterandacetonitrileasmobilephaseswithgradientelution.Theidentificationofamoxicil
7、linwascarriedoutbyMS/MSequippedwithelectrosprayionizationinpositivescanningandmultiplereactionmonitoring(MRM)modes.【Resultandconclusion】Matrix-matchedcalibrationstandardwasusedforthequantification.Thecalibrationcurve-1showedperfectlinearityintherangeof1-400μg·L,witht
8、hecorrelationcoefficientbeingmorethan收稿日期:2013-02-21优先出版时间:2014-06-03优先出版网址:http:∥www.cnki.net/kcms/doi/10.7671/j.issn.1001-411X.20
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