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目的建立同时测定全血中溴鼠隆、溴敌隆、氟鼠灵、杀鼠灵和鼠得克5种灭鼠剂的高效液相色谱测定方法。方法取0.5 m L全血样品经2.0 m L乙酸乙酯萃取后,采用Diamonsil C18(250.0 mm×4.6 mm×5.0μm)色谱柱分离,以浓度为20 mmol/L的乙酸铵-乙酸缓冲液(p H值=5.5)∶甲醇(2∶8,V/V)为流动相,在二极管阵列检测器检测波长为310 nm的紫外光谱下经高效液相色谱仪测定。结果全血中溴鼠隆、溴敌隆、氟鼠灵、杀鼠灵和鼠得克在质量浓度为0.50~10.00 mg/L线性关系良好,相关系数均大于0.999 00,检出限分别为0.08、0.06、0.09、0.04和0.10 mg/L,定量下限分别为0.79、0.58、0.92、0.45和0.96 mg/L。加标回收率为98.40%~104.00%。批内相对标准偏差为0.61%~7.84%,批间相对标准偏差为1.10%~9.62%。样品在4℃冰箱内可保存14 d。结论本方法操作简单、分离效果好、灵敏度高,具有较好的精密度和准确度,适用于灭鼠剂中毒患者全血样品的检测。
OBJECTIVE To establish a method for simultaneous determination of 5 rodenticides in rat blood by bromodextrole, bromadiolone, fluoxetine, warfarin and dimethoate. Methods 0.5 mL whole blood samples were extracted with 2.0 mL ethyl acetate and separated on a Diamonsil C18 column (250.0 mm × 4.6 mm × 5.0 μm). The cells were eluted with 20 mmol / L ammonium acetate-acetate buffer ( p H = 5.5): methanol (2: 8, V / V) was used as the mobile phase and detected by HPLC using a diode array detector at a UV detection wavelength of 310 nm. Results The linearity of bromodextrine, bromadiolone, fluoxetine, warfarin and dimethodextrin in whole blood was good in the range of 0.50-10.00 mg / L. The correlation coefficients were all above 0.999 00 with the detection limits of 0.08 , 0.06,0.09,0.04 and 0.10 mg / L, respectively. The lower limits of quantitation were 0.79, 0.58, 0.92, 0.45 and 0.96 mg / L, respectively. Spike recovery was 98.40% ~ 104.00%. The relative standard deviations in the batch ranged from 0.61% to 7.84%, and the relative standard deviations in the batch ranged from 1.10% to 9.62%. Samples can be stored in a refrigerator at 4 ℃ for 14 days. Conclusion The method has the advantages of simple operation, good separation effect, high sensitivity, good precision and accuracy, and is suitable for the detection of whole blood samples in patients with rodenticide poisoning.