动物医学进展
動物醫學進展
동물의학진전
PROGRESS IN VETERINARY MEDICINE
2014年
9期
85-89
,共5页
刘静%郑增忍%赵思俊%曲志娜%王君玮%孙晓亮%谭维泉%刘坤%曹旭敏%邹明
劉靜%鄭增忍%趙思俊%麯誌娜%王君瑋%孫曉亮%譚維泉%劉坤%曹旭敏%鄒明
류정%정증인%조사준%곡지나%왕군위%손효량%담유천%류곤%조욱민%추명
超高效液相色谱-串联质谱%青霉素G%青霉噻唑酸%牛奶
超高效液相色譜-串聯質譜%青黴素G%青黴噻唑痠%牛奶
초고효액상색보-천련질보%청매소G%청매새서산%우내
UPLC-MS/MS%penicillin G%benzylpenicillin acid%milk
为建立同时检测牛奶中青霉素 G 及青霉噻唑酸的 UPLC-MS/MS 检测法，将牛奶样品经乙腈∶乙醇（3∶1，V∶V）提取后离心分离，用 Oasis HLB 固相萃取柱净化，进行超高效液相色谱-串联质谱法检测。青霉素和青霉噻唑酸在线性范围内相关系数在0．993以上，方法的检出限（LOD，S/N＝3）为0．3μg/kg～0．5μg/kg，定量限（S/N＝10）为1．0μg/kg～2．0μg/kg。选用基质添加标准曲线消除基质干扰，样品加标回收率为75．88％～106．01％，变异系数为6．65％～14．17％。说明方法的灵敏度高，重复性良好，为快速准确的检测该类药物提供可靠的技术支撑。
為建立同時檢測牛奶中青黴素 G 及青黴噻唑痠的 UPLC-MS/MS 檢測法，將牛奶樣品經乙腈∶乙醇（3∶1，V∶V）提取後離心分離，用 Oasis HLB 固相萃取柱淨化，進行超高效液相色譜-串聯質譜法檢測。青黴素和青黴噻唑痠在線性範圍內相關繫數在0．993以上，方法的檢齣限（LOD，S/N＝3）為0．3μg/kg～0．5μg/kg，定量限（S/N＝10）為1．0μg/kg～2．0μg/kg。選用基質添加標準麯線消除基質榦擾，樣品加標迴收率為75．88％～106．01％，變異繫數為6．65％～14．17％。說明方法的靈敏度高，重複性良好，為快速準確的檢測該類藥物提供可靠的技術支撐。
위건립동시검측우내중청매소 G 급청매새서산적 UPLC-MS/MS 검측법，장우내양품경을정∶을순（3∶1，V∶V）제취후리심분리，용 Oasis HLB 고상췌취주정화，진행초고효액상색보-천련질보법검측。청매소화청매새서산재선성범위내상관계수재0．993이상，방법적검출한（LOD，S/N＝3）위0．3μg/kg～0．5μg/kg，정량한（S/N＝10）위1．0μg/kg～2．0μg/kg。선용기질첨가표준곡선소제기질간우，양품가표회수솔위75．88％～106．01％，변이계수위6．65％～14．17％。설명방법적령민도고，중복성량호，위쾌속준학적검측해류약물제공가고적기술지탱。
An ultra performance liquid chromatography tandem mass spectrometric (UPLC-MS/MS)anal-ysis method was established for simultaneous analysis of penicillin G and benzylpenicillin acid in milk.The milk samples were precipitated with acetonitrile:alcohol(3 ∶ 1,V∶ V),and the extracts were applied to HLB cartridge for clean up,the separation was performed by ultra performance liquid chromatography-tan-dem mass spectrometry.The correlation coefficients were above 0.993.The detection limits (S/N>3)of penicillin acid G and benzylpenicillin acid were 0.3 μg/kg-0.5 μg/kg.The detection limits (S/N>10)of penicillin G and benzylpenicillin were 1.0 μg/kg-2.0 μg/kg.The results quantified by matrix spiked cali-bration curve,the recoveries ranged from 75.88%-106.0%,and RSD were in the range of 6.65%-14.17%. The method is sensitive and repeatable,and can be applied to the field of residue analysis about penicillin and their metabolites.
