摘要
目的：通过对超高效液相色谱法条件的筛选,建立了超高效液相色谱-四极杆串联质谱仪检测头孢噻呋在大鼠乳腺组织中残留量的方法。方法：大鼠乳腺组织经乙腈水溶液提取,浓缩后经固相萃取、净化、反相液相色谱分离后进行质谱分析,在多反应监测模式（MRM）下进行特征母-子离子对信号采集。根据保留时间对母离子和两个特征子离子的离子信息进行定性分析,以丰度最大的子离子m/z 241进行定量分析。结果：最低检测限（S/N=3）为0.1ng/g,定量限为0.5ng/g,在1.0~20.0ng/g时峰面积与质量浓度的线性关系良好（r=0.9992,n=6）。在1.0,5.0,10.0ng/g 3个添加水平,平均回收率范围为97.85%,测定结果的相对标准偏差小于7%。结论：该方法简单、特异性强、灵敏度高、分析时间短,适用于乳腺组织中头孢噻呋残留定性分析和定量检测。
A confirmative method of ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry（ UPLC- ESI- MS / MS） for detecting the ceftiofur residues in the galactophore tissue of rat was established. The sample was extracted by acetonitrile- water and concentrated. And the ceftiofur was isolated and purified from diluted samples by solid- phase extraction. Following reversed- phase liquid chromatography separation,mass spectral acquisition of two diagnostic transition reactions was applied with multiple reaction monitoring mode. The qualitative analysis was performed by basis on the retention time,the precursor ion and two product ions,and the quantitative analysis was carried out with intension of the characteristic ion m / z 241. The method detection limit and quantitation limit was 0. 1ng / g and 0. 5ng / g,respectively. The linear ranges were from 1. 0ng / g to 20 ng /g for ceftiofur and the correlation coefficient was greater than 0. 996. The average recovery was 97. 85% in replicate sets of the tissue of galactophore samples spiked with the drug concentrations of 1. 0,5. 0 and 10. 0ng / g,and the relative standard deviations（ RSD）was less than 7%. Therefore,the established method is simple and suitable methods for routine analysis with high specificity and sensitivity,need comparatively short time for analysis,and suitable for applying in qualitative analysis and quantitative analysis ceftiofur residue in galactophore samples.
出处
《内蒙古农业大学学报（自然科学版）》
CAS
2015年第3期1-5,共5页
Journal of Inner Mongolia Agricultural University(Natural Science Edition)
基金
内蒙古自治区自然科学基金(2012MS0424)
