Liu Xiangguo, Su Yijuan, Fang Binghu, Ding Huanzhong, He Limin, Zeng Zhenling, Chen Zhangliu
Department of Pharmacology and Toxicology, College of Veterinary Medicine, South China Agricultural University, Guangzhou 510642, China.
Se Pu. 2009 Jan;27(1):86-90.
A confirmative method to determine clopidol residues in chicken muscle by gas chromatography-mass spectrometry (GC-MS) was developed. The analyte was extracted with ace tonitrile, and then purified with an Alumina-B cartridge column. The drug was derived at 80 degrees 3 for 60 min with Sylon BFT, and more toluene was added and then applied to GC-MS. The mass spectral characteristics of trimethylsilyl derivative of clopidol were interpreted, and selected ion monitoring (SIM) mode was performed at m/z 212, 214, 248 and 263. The clopidol was qualitatively identified by the ratio of relative abundance of the selected ions and determined quantitatively by SIM mode at m/z 248. In the meantime, the matrix effect was evaluated. The range of linearity was 5.0 - 500 microg/L with the correlation coefficients better than 0.998, and the detection limit was 0.5 microg/kg (S/N = 3) for clopidol. The average recoveries from chicken muscle fortified at 5, 10 and 20 microg/kg were 77.0%, 84.5% and 89.4%, respectively, and the relative standard deviations (RSD) were less than 6.9%. The established method is simple, sensitive and reproducible for the identification and quantification of clopidol residues in chicken muscle tissue.
建立了一种用气相色谱-质谱联用仪(GC-MS)测定鸡肉中氯羟吡啶残留量的确证方法。用乙腈提取分析物,然后用氧化铝-B柱净化。药物在80℃下用Sylon BFT衍生化60分钟,加入更多甲苯后进行GC-MS分析。解析了氯羟吡啶三甲基硅烷基衍生物的质谱特征,并在m/z 212、214、248和263处采用选择离子监测(SIM)模式。通过选择离子的相对丰度比定性鉴定氯羟吡啶,并在m/z 248处用SIM模式进行定量测定。同时,评估了基质效应。线性范围为5.0 - 500μg/L,相关系数优于0.998,氯羟吡啶的检出限为0.5μg/kg(S/N = 3)。在5、10和20μg/kg加标水平下,鸡肉中的平均回收率分别为77.0%、84.5%和89.4%,相对标准偏差(RSD)小于6.9%。所建立的方法用于鸡肉组织中氯羟吡啶残留的鉴定和定量分析,具有简单、灵敏和可重复的特点。