摘要
研究建立灵敏、可靠的同时检测猪肉组织中氯霉素（CAP）、甲砜霉素（TAP）及氟甲砜霉素（FF）残留的气质联用方法。通过优化气相色谱条件，实现了氯霉素、甲砜霉素及氟甲砜霉素三甲基硅衍生物的良好分离；对氯霉素、甲砜霉素及氟甲砜霉素三甲基硅醚峰的质谱碎片进行了归属；选择监测离子：氯霉素（m／z225、242、244、361）。氟甲砜霉素（178、257、259、394）及甲砜霉素（242、244、257、330）作为定性定量的依据。试样采用乙腈提取，C18固相小柱纯化，Sylon BFT在80℃衍生30min。3种兽药衍生物的峰面积与其质量浓度在CAP为2．00，1000μg/L，FF与TAP为5．00—1000μg/L时成线性关系，线性回归系数均大于0．999。方法检出限：CAP达1．0μg/kg，FF及TAP为2．0μg／kg。猪肉组织在10μg／kg水平添加标准，CAP、FF与TAP平均回收率分别88％、78％和81％．相对标准偏差分别为7．7％、10．5％和8．1％。
A reproducible, sensitive method to determine fenicols residues in pork by gas chromatography- mass spectrometry（ GC -MS） was developed for the need to monitor animal food. TMS derivatives of fenieols were separated through optimizing the gas chromatographic - mass spectrometric conditions. Mass spectral characteristics of TMS derivatives of ehloramphenieol （ CAP）, florfenicol （ FF）, and thiamphenieol（TAP） were interpreted, respectively. Mass spectral analysis was performed in the selected ion monitoring mode at m/z 225, 242, 244, and 361 for CAP, 178, 257, 259, and 394 for FF, and 242, 244, 257, and 330 for TAP. The composite sample was extracted with aeetonitrile, and applied to a C18 cartridge successively. The drug was derivatized at 80 ℃ for 30 min with Sylon BFT. The method detection limits were about 1.0 μg/kg for CAP and 2.0 μg/kg for FF and TAP.
出处
《分析测试学报》
CAS
CSCD
北大核心
2006年第2期43-46,51,共5页
Journal of Instrumental Analysis
关键词
氯霉素类三甲基硅醚
质谱表征
气质联用
猪组织
兽药残留
Fenicols TMS ether
Mass spectral characteristics
GC - MS
Pork tissues
Phenicols residues
