高效液相色谱法测定全血中5种抗凝血类灭鼠剂

发布时间：2018-05-04 07:51

  本文选题：抗凝血灭鼠剂 + 溴鼠隆　； 参考：《中国职业医学》2016年02期

【摘要】：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。
[Abstract]:Objective to establish a high performance liquid chromatography (HPLC) method for the simultaneous determination of brominolone, bromadiolone, flurazone, shayanling and Rutake in whole blood. Methods 0.5 mL whole blood samples were extracted with 2.0 mL ethyl acetate and separated by Diamonsil C180.0 mm 脳 4.6 mm 脳 5.0 渭 m column. The mobile phase consisted of 20 mmol/L ammonium acetate buffer solution with pH value of 5.5%: methanol 2: 8 V / V). The UV spectrum at 310 nm was determined by high performance liquid chromatography (HPLC) with diode array detector. Results there was a good linear relationship between brominolone, bromadiolone, flurazone, shayanling and Rutecke in whole blood. The correlation coefficient was more than 0.999 mg/L, the detection limits were 0.08%, 0.09 mg / L and 0.10 mg / L, respectively, and the lower limit of quantification was 0.790.580.92% 0.45 and 0.96 mg 路L ~ (-1) 路L ~ (-1), and the limit of detection was 0.08 mg / L and 0.10 mg 路L ~ (-1), respectively. The recovery rate was 98.40% and 104.00%. The relative standard deviation (RSD) was 0.61% 7.84, and the relative standard deviation between batches was 1.10% and 9.62%, respectively. The sample can be stored in 4 鈩，

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