兽用抗生素中非法添加5种解热镇痛类药物的高效液相色谱检测方法研究

建立兽用抗生素注射液与可溶性粉剂中非法添加对乙酰氨基酚、安乃近、安替比林、萘普生、氨基比林5种药物的高效液相色谱—二极管阵列检测分析方法。样品经甲醇超声提取后进行液相色谱分析,采用CAPCELL PAK MG C18(4.6 mm×250 mm,5μm)色谱柱,柱温30℃,流动相为乙腈和磷酸盐缓冲液,梯度洗脱,检测波长229 nm,流速1.0 m L/min。对乙酰氨基酚、安乃近、安替比林、萘普生、氨基比林进样量分别在5.04~100.88、12.04~240.72、5.04~100.72、2.02~40.40、5.02~100.32μg/m L范围内呈良好的线性关系;平均加样回收率(n=5)分别为97.9%~102.8%、91.9%~98.8%、96.2%~101.1%、94.1%~102.3%、96.0%~102.8%,RSD分别为1.0%~3.1%、0.9%~6.4%、1.7%~4.2%、1.4%~3.9%、0.9%~4.8%。该方法快捷、简便,其准确性和灵敏度经方法学验证能很好地满足检测多种抗生素中非法添加解热镇痛类药物的筛查要求。

Simultaneous Determination of Five Kinds of Antipyretic Analgesic Drugs Illegally Added into Veterinary Antibiotics by HPLC-DAD

A high-performance liquid chromatography （HPLC）-photodiode array detector （DAD） method was established for determination of paracetamol, dipyrone, phenazone, naproxen, aminopyrine illegally added into veterinary antibiotics injection and soluble powder. Samples were extracted under uhrasonication with methanol. A CAPCELL PAK MG Cis analytical column （4.6 mm ×250 mm, 5 μm） was used for the column temperature was at 30 ℃ and the detection wavelength was set at 229 nm. Acetonitrile-phosphate buffer was used as the mobile phase under the program of gradient elution at a flow rate of 1.0 mL/min. The calibration curves of paracetamol, dipyrone, phenazone, naproxen and aminopyrine showed good linearity in the ranges of 5.04-100.88, 12.04-240.72, 5.04-100.72, 2.02-40.40 and 5.02-100.32 μg/mL. The average recoveries （n=5） were 97.9%- 102.8%, 91.9%-98.8%, 96.2%-101.1%, 94.1%-102.3% and 96.0%-102.8%, and RSDs were 1.0%-3.l%, 0.9%-6.4%, 1.7%-4.2%, 1.4%-3.9% and 0.9%-4.8%, respectively. The methodology validation showed that this method was simple, accurate and reliable, so it was appropriate for the determination of the antipyretic analgesic drugs in many kinds of veterinary antibiotics.