HPLC-DAD法测定2种中兽药散剂中非法添加非泼罗尼
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摘要
建立鸡球虫散、驱虫散中非法添加非泼罗尼的液相色谱检查方法。采用Agilent Eclipse Plus-C_(18)(3.5μm,4.6 mm×100 mm)色谱柱,以乙腈-水为流动相,梯度洗脱,二极管阵列检测器,波长采集190～400 nm,检查波长220 nm。通过色谱峰保留时间、峰纯度检查和光谱相似度检查对非泼罗尼进行定性,通过峰面积外标法进行定量。结果表明,方法检测限(LOD)为0.25 g/kg,在0.5 g/kg、2.0 g/kg、5.0 g/kg 3个添加浓度下,平均回收率为95.4%～101.5%,相对标准偏差为1.5%～2.5%,能够满足实际需求。本方法操作简单、检测快速、结果可靠,适用于以上2种制剂中非法添加非泼罗尼的定性定量检测。
The detection method of fipronil illegally addition in Jiqiuchongsan(medicine against chicken coccidiosis) and quchongsan(vermifuge) was established by HPLC-DAD. The isolation was performed on the Agilent Eclipse Plus-C_(18)(3.5μm,4.6×100 mm)chromatogramcolumn,gradient elution was carried out with water-acetonitrile as mobile phase. Used the diode array detector,The extraction wavelength was 220 nm. Fiproni was quantified by the retention time of chromatographic peak,peak purity testand spectra similarity,fiproni was quantitated by peak area. The results showed that the LOD was 0.25 g/kg,the average recovery rate ranged from 95.4 % ～ 101.5% at the level of 0.5,2.0,and 5.0 g/kg,the RSD was 1.5%～2.5%. This method was simple,fast and reliable,couldbe used as the determination method of quality and quantity.
The detection method of fipronil illegally addition in Jiqiuchongsan(medicine against chicken coccidiosis) and quchongsan(vermifuge) was established by HPLC-DAD. The isolation was performed on the Agilent Eclipse Plus-C_(18)(3.5μm,4.6×100 mm)chromatogramcolumn,gradient elution was carried out with water-acetonitrile as mobile phase. Used the diode array detector,The extraction wavelength was 220 nm. Fiproni was quantified by the retention time of chromatographic peak,peak purity testand spectra similarity,fiproni was quantitated by peak area. The results showed that the LOD was 0.25 g/kg,the average recovery rate ranged from 95.4 % ～ 101.5% at the level of 0.5,2.0,and 5.0 g/kg,the RSD was 1.5%～2.5%. This method was simple,fast and reliable,couldbe used as the determination method of quality and quantity.
引文
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[11]魏秀丽,张传津,李有志.UPLC-PDA法测定杨树花口服液中非法添加物黄芩苷[J].中国兽药杂志,2018,52(1):50-55.
[2]曹明章.氟虫腈对四种贮粮害虫的杀虫效果:贮粮种类、剂量、接触时间、相对湿度和温度的影响[J].世界农药,2010,32(6):36-39+45.
[3]周彤,肖洪喜,周志俊.氟虫腈安全性评价资料概述[J].环境与职业医学,2017,34(08):745-748.
[4]何国鑫,林锡芳,刘晓,等.氟虫腈急性中毒小鼠毒性和病理形态学改变[J].温州医学院学报,2005(3):179-181.
[5]吕磊.水产品中敌敌畏和氟虫腈的残留研究[D].武汉:华中农业大学,2013.
[6]Kairo G,Biron DG,Ben AF,et al.Nosema ceranae,Fipronil and their combination compromise honey bee reproduction via changes in malephysiology[J].Sci Rep,2017,7(1):8556.
[7]魏秀丽,张传津,李有志.UPLC-PDA法测定杨树花口服液中非法添加物黄芩苷[J].中国兽药杂志,2018,52(1):50-55.
[8]杨修镇,陈玲,尹伶灵,等.液相色谱-串联质谱法测定阿维菌素粉中非法添加非泼罗尼的研究[J].中国兽药杂志,2018,52(4):32-37.
[9]田晓玲.HPLC法测定中兽药散剂中非法添加的10种磺胺类药物[J].现代畜牧兽医,2018(7):16-19.
[10]张航俊,周芷锦,侯轩,等.HPLC-MS/MS检测双黄连注射液中非法添加13种喹诺酮类药物的研究[J].中国兽药杂志,2016,50(12):59-64.
[11]魏秀丽,张传津,李有志.UPLC-PDA法测定杨树花口服液中非法添加物黄芩苷[J].中国兽药杂志,2018,52(1):50-55.