Xu Daokun, Huang Haolun, Hu Wenyan, Liu Xinmei, Yang Jun
Nanjing Institute for Food and Drug Control, Nanjing, 211198, Jiangsu Province, People's Republic of China.
State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi, 214122, Jiangsu Province, People's Republic of China.
BMC Chem. 2023 Aug 7;17(1):96. doi: 10.1186/s13065-023-01010-4.
A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the analysis of ribavirin in chicken. Samples was extracted with 0.1% formic acid and purified by Hypercarb cartridge prior to LC-MS/MS analysis. The eluates were evaporated to dryness, reconstituted in 1 mL 5mM ammonium acetate containing 5% acetonitrile (v/v) and 0.1% (v/v) formic acid. Chromatographic separation was performed on a Hypercarb analytical column under a gradient elution program with acetonitrile and 0.1% (v/v) formic acid in 5 mM ammonium acetate at a flow rate of 0.6 ml/min. The intraday and interday accuracy ranged from - 7.83 - 1.39%, and - 6.38 - 2.25%, with precisions between 1.34 - 3.88%% and 1.10 - 4.67%. The limits of detection (LODs) and limits of quantitation (LOQs) of ribavirin was 0.1 ng/mL and 0.5 ng/mL, respectively. The method was validated for linearity, accuracy, precision, matrix effect and stability. Application of the method confirmed 3 ribavirin positive samples out of 50 commercial chicken samples, with concentrations of ribavirin ranging from 0.9 μg/kg to 5.8 μg/kg a, respectively. Additionally, both AB Sciex 5500 and Agilent 6945B were proven to be suitable in ribavirin separation and quantification. The described method is suitable for the determination of ribavirin in chicken in analytical practice to monitor illegal addition of this kind of anti-viral drug.
建立了一种液相色谱-串联质谱（LC-MS/MS）法用于分析鸡肉中的利巴韦林。样品用0.1%甲酸提取，在进行LC-MS/MS分析之前通过Hypercarb柱净化。洗脱液蒸发至干，用含5%乙腈（v/v）和0.1%（v/v）甲酸的1 mL 5 mM乙酸铵复溶。在Hypercarb分析柱上按照梯度洗脱程序进行色谱分离，流动相为乙腈和含0.1%（v/v）甲酸的5 mM乙酸铵，流速为0.6 ml/min。日内和日间准确度范围分别为-7.83%至1.39%和-6.38%至2.25%，精密度分别在1.34%至3.88%和1.10%至4.67%之间。利巴韦林的检测限（LOD）和定量限（LOQ）分别为0.1 ng/mL和0.5 ng/mL。该方法在线性、准确度、精密度、基质效应和稳定性方面得到了验证。应用该方法在50份市售鸡肉样品中确认了3份利巴韦林阳性样品，利巴韦林浓度分别为0.9 μg/kg至5.8 μg/kg。此外，AB Sciex 5500和安捷伦6945B均被证明适用于利巴韦林的分离和定量。所描述的方法适用于分析实践中鸡肉中利巴韦林的测定以监测此类抗病毒药物的非法添加。
