高效液相色譜法測(cè)定全血中5種抗凝血類滅鼠劑
發(fā)布時(shí)間:2018-05-04 07:51
本文選題:抗凝血滅鼠劑 + 溴鼠隆。 參考:《中國(guó)職業(yè)醫(yī)學(xué)》2016年02期
【摘要】:目的建立同時(shí)測(cè)定全血中溴鼠隆、溴敵隆、氟鼠靈、殺鼠靈和鼠得克5種滅鼠劑的高效液相色譜測(cè)定方法。方法取0.5 m L全血樣品經(jīng)2.0 m L乙酸乙酯萃取后,采用Diamonsil C18(250.0 mm×4.6 mm×5.0μm)色譜柱分離,以濃度為20 mmol/L的乙酸銨-乙酸緩沖液(p H值=5.5)∶甲醇(2∶8,V/V)為流動(dòng)相,在二極管陣列檢測(cè)器檢測(cè)波長(zhǎng)為310 nm的紫外光譜下經(jīng)高效液相色譜儀測(cè)定。結(jié)果全血中溴鼠隆、溴敵隆、氟鼠靈、殺鼠靈和鼠得克在質(zhì)量濃度為0.50~10.00 mg/L線性關(guān)系良好,相關(guān)系數(shù)均大于0.999 00,檢出限分別為0.08、0.06、0.09、0.04和0.10 mg/L,定量下限分別為0.79、0.58、0.92、0.45和0.96 mg/L。加標(biāo)回收率為98.40%~104.00%。批內(nèi)相對(duì)標(biāo)準(zhǔn)偏差為0.61%~7.84%,批間相對(duì)標(biāo)準(zhǔn)偏差為1.10%~9.62%。樣品在4℃冰箱內(nèi)可保存14 d。結(jié)論本方法操作簡(jiǎn)單、分離效果好、靈敏度高,具有較好的精密度和準(zhǔn)確度,適用于滅鼠劑中毒患者全血樣品的檢測(cè)。
[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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