超高效液相色谱-串联质谱法测定中兽药散剂中4种喹诺酮药物

Determination of four quinolone drugs in veterinary traditional Chinese medicine powders by ultra performance liquid chromatography-tandem mass spectrometry

为了检测中兽药散剂中喹诺酮类药物的非法添加情况,试验利用超高效液相色谱-串联质谱技术,采用ACQUITY UPLCTM C18色谱柱(2.1 mm×100 mm)进行分离,以乙腈(A)和0.2%甲酸溶液(B)为流动相,梯度洗脱,多反应监测(MRM)扫描,电喷雾电离正离子模式(ESI+),流速为0.4 m L/min,外标法定量。结果表明:4种喹诺酮药物在1~100 ng/m L浓度范围内,药物浓度与吸收峰面积呈现良好的线性关系,相关系数(r)≥0.997。检出限为0.3 ng/m L,定量限为1 ng/m L。该方法可以同时定量检测中兽药散剂中是否添加4种喹诺酮类药物,具有快速、准确、灵敏、成本较低、节省时间、可以应用于高通量的实际检测样品等优点。

To detect the illegal addition of quinolones in veterinary traditional Chinese medicine powders, a method was established by using ul- tra performance liquid chromatography- tandem mass spectrometry. ACQUITY UPLCTMC18 （2.1 mm × 100 mm） chromatographic column was used for separation process, and acetonitrile （A） and 0.2 % formic acid solution （B） were used as the mobile phase with gradient elution at the flow rate of 0.4 mL/min. Quinolone drugs were detected with multiple reaction monitoring （MRM） scanning with positive ion mode electrospray ionization （ ESI ＋ ） , and external standard method were employed for quantification. The results showed that there was a good linear relationship between drug concentration and absorption peak area in the concentration range from 1 to 100 ng/mL for four quinolones, and the correlation co- efficient was greater than or equal to 0. 997, the detection limit was 0.3 ng/mL, and the quantification limit was 1 ng/mL. The results indicate that the method can simultaneously quantitatively detect whether or not four quinolones are added in veterinary traditional Chinese medicine pow- ders, which has the advantages of rapidity, accuracy, sensitivity, low cost, time saving, and can be used for actual test samples of high output and so on.