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目的建立二极管阵列检测器串联荧光检测器测定血浆中杀鼠酮、华法灵、杀鼠醚、氯杀鼠灵、敌鼠、氯鼠酮、溴敌隆、大隆的超高效液相色谱法。方法血浆样品经固相萃取净化提取后,采用Hypersil BDS C18(100 mm×4.6 mm,2.4μm)色谱柱分离,用甲醇-0.04 mol/L乙酸铵缓冲液(42∶58,V/V)进行梯度洗脱,流速为1.0 ml/min,同时用二极管阵列检测器和荧光检测器检测杀鼠酮、华法灵、杀鼠醚、氯杀鼠灵、敌鼠、氯鼠酮、溴敌隆、大隆。结果 8种抗凝血类杀鼠剂用二极管阵列检测器检测,在0.02 mg/L~5.0 mg/L有良好的线性关系;用荧光检测器检测,在0.01 mg/L~3.0 mg/L有良好的线性关系,r为0.998 6~0.999 2,平均加标回收率为74.2%~111.2%,相对标准偏差为2.9%~8.8%。结论该方法快速、简单,可应用于血浆中抗凝血类杀鼠剂的检测。
OBJECTIVE To establish a diode-array detector tandem fluorescence detector for the determination of nematicolamine, warfarin, warfarin, clomipramine, warfarin, clomiphene, bromadiolone and daron in plasma by ultra performance liquid chromatography . Methods The plasma samples were purified by solid-phase extraction and then separated on a Hypersil BDS C18 (100 mm × 4.6 mm, 2.4 μm) column with methanol-0.04 mol / L ammonium acetate buffer (42:58, V / V) Gradient elution at a flow rate of 1.0 ml / min, while using a diode array detector and a fluorescence detector to detect naloxone, warfarin, warfarin, chlorine warfarin, dipyridamole, Dalong. Results Eight anticoagulant rodenticides were detected by diode array detector with a good linearity at 0.02 mg / L ~ 5.0 mg / L. Fluorescence detector was used to detect the concentration of oxaliplatin between 0.01 mg / L and 3.0 mg / L Good linear relationship, r is 0.998 6 ~ 0.999 2, the average recovery of 74.2% ~ 111.2%, the relative standard deviation of 2.9% to 8.8%. Conclusion The method is rapid and simple and can be applied to the detection of anticoagulant rodenticides in plasma.