3种固相萃取柱在测定牛血清样品中乙酰氨基阿维菌素前处理中的比较研究
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摘要
初步评价在乙酰氨基阿维菌素药动学前处理中3种固相萃取柱对乙酰氨基阿维菌素的净化、萃取效果。首先在空白胎牛血清中加入一定量的乙酰氨基阿维菌素标准溶液,经色谱甲醇提取后,分别经Agilent公司、Waters公司和Agela Technologies公司的C_(18)SPE柱进行萃取(分别简称A固相萃取柱、W固相萃取柱、AT固相萃取柱),再经N-甲基咪唑和三氟乙酸酐衍生化,最后用超高效液相色谱-荧光检测器进行测定。与此同时,将等量的乙酰氨基阿维菌素标准溶液进行衍生化,用超高效液相色谱-荧光检测器进行测定,其结果作为对照。以绝对回收率作为评价3种SPE柱净化、萃取EPR效果的标准。结果显示,含有EPR的胎牛血清经A固相萃取柱萃取后,EPR峰形尖锐对称且无明显杂质峰,其绝对回收率为80.79%;经W固相萃取柱萃取后,乙酰氨基阿维菌素峰形尖锐对称且无明显杂质峰,其绝对回收率为83.61%;经AT固相萃取柱萃取后,乙酰氨基阿维菌素峰形尖锐对称且无明显杂质峰,其绝对回收率仅为64.20%。相对于A与AT固相萃取柱,Waters公司的C_(18)SPE柱萃取EPR的效果更好。研究结果为后期乙酰氨基阿维菌素的药物代谢动力学试验奠定了基础。
In order to preliminarily evaluate the purification and extraction effects of eprinomectin on the three solid phase extraction columns in the pharmacokinetic pretreatment of eprinomectin,firstly,a certain amount of eprinomectin standard solution was added to blank fetal bovine serum.Methanol was used to extracte EPR in serum.Then,solution was extracted by Agilent,Agela Technologies and Waters C_(18)SPE column,and it was derivatized with N-methylimidazole and trifluoroacetic anhydride.The final product was determined by ultra performance liquid chromatography-fluorescence detector.At the same time,an equal amount of eprinomectin standard solution was derivatized directly with N-methylimidazole and trifluoroacetic anhydride.The final product was determined by ultra performance liquid chromatography-fluorescence detector.The final result was taken as the control group.The evaluation criterion is the absolute recovery rate.The results showed that the EPR containing fetal bovine serum was extracted by Agilents solid phase extraction column,and the EPR peak shape was sharp and symmetric without obvious impurity peaks.The absolute recovery was 80.79%.The EPR peak shape was sharp and symmetric,and there was no obvious impurity peak after extraction by Waterss solid-phase extraction column.The absolute recovery was83.61%.The EPR peak shape was sharp and symmetric without obvious impurity peaks after extraction by Agela Technologiess solid-phase extraction column and its absolute recovery was only 64.20%.WatersC_(18)SPE column has better extraction of EPR compared to the other companies'solid phase extraction columns.This study laid a good foundation for the later animal pharmacokinetics test.
In order to preliminarily evaluate the purification and extraction effects of eprinomectin on the three solid phase extraction columns in the pharmacokinetic pretreatment of eprinomectin,firstly,a certain amount of eprinomectin standard solution was added to blank fetal bovine serum.Methanol was used to extracte EPR in serum.Then,solution was extracted by Agilent,Agela Technologies and Waters C_(18)SPE column,and it was derivatized with N-methylimidazole and trifluoroacetic anhydride.The final product was determined by ultra performance liquid chromatography-fluorescence detector.At the same time,an equal amount of eprinomectin standard solution was derivatized directly with N-methylimidazole and trifluoroacetic anhydride.The final product was determined by ultra performance liquid chromatography-fluorescence detector.The final result was taken as the control group.The evaluation criterion is the absolute recovery rate.The results showed that the EPR containing fetal bovine serum was extracted by Agilents solid phase extraction column,and the EPR peak shape was sharp and symmetric without obvious impurity peaks.The absolute recovery was 80.79%.The EPR peak shape was sharp and symmetric,and there was no obvious impurity peak after extraction by Waterss solid-phase extraction column.The absolute recovery was83.61%.The EPR peak shape was sharp and symmetric without obvious impurity peaks after extraction by Agela Technologiess solid-phase extraction column and its absolute recovery was only 64.20%.WatersC_(18)SPE column has better extraction of EPR compared to the other companies'solid phase extraction columns.This study laid a good foundation for the later animal pharmacokinetics test.
引文
[1]石奥.固相萃取-超高效液相色谱-串联质谱法测定畜禽饮用水中23种抗生素和3种β-受体激动剂[J].色谱,2016,34(2):176-183.
[2]杨二爽,李小莲,沈雁,等.高效液相色谱法测定乙酰氨基阿维菌素的含量[J].黑龙江畜牧兽医,2017(12):162-164.
[3]刘永涛,余琳雪,王桢月,等.改良的QuEChERS结合高效液相色谱-串联质谱同时测定水产品中7种阿维菌素类药物残留[J].色谱,2017,35(12):1276-1285.
[4]李建华,刘琴,周亚平,等.乙酰氨基阿维菌素对奶牛寄生虫治疗效果评价实验[J].中国畜牧兽医文摘,2018,34(2):254-241.
[5]都倩.多沙唑嗪的SPE-LC-MS/MS分析方法建立及其在大鼠体内代谢的研究[D].河石家庄北:河北医科大学,2017.
[6]丁杨,邓美荣,聂晶,等.固相萃取-高效液相色谱法测定乳制品中三聚氰胺的含量[J].中国卫生工程学,2016,15(1):41-45.
[7]冒玉娟,陈晓兰,赵丽.乙酰氨基阿维菌素在动物医学中的研究进展[J].畜牧与饲料科学,2013,34(1):86-89.
[8]Pollock J,Bedenice D,Jennings S H,et al.Pharmacokinetics of an extended-release formulation of eprinomectin in healthy adult alpacas and its use in alpacas confirmed with mange[J].J Vet pharmacol Ther,2017,40(2):192-199.
[9]Brique-Pellet C,Ravinet N,Quenet Y,et al.Pharmacokinetics and anthelmintic efficacy of injectable eprinomectin in goats[J].Vet Parasitol,2017,241(10):43-47.
[10]Lifschitz A,Nava S,Mangold A,et al.Eprinomectin accumulation in Rhipicephalus(Boophilus)microplus:Pharmacokinetic and efficacy assessment[J].Vet Parasitol,2016,215(2):11-16.
[11]高三玉,周芷锦,罗成江,等.高效液相色谱法测定牛奶中乙酰氨基阿维菌素的残留量[J].畜牧与饲料科学,2017,38(4):14-16.
[12]Wang Q,Zhao R,Cui Y,et al.Rapid and simple determination of sarafloxacin and difloxacin in beef by capillary electrophoresis coupled with solid-phase extraction[J].J Anal Methods Chem,2018,2018(8):19-36.
[13]Gokbulut C,Ozuicli M,Aksit D,et al.Comparative plasma and milk dispositions,faecal excretion and efficacy of per os ivermectin and pour-on eprinomectin in horses[J].J Vet Pharmacol Ther,2016,39(6):584-589.
[14]任丽君,郭玉娟,姚军,等.伊维菌素缓释注射液的制备工艺及在绵羊体内药代动力学研究[J].西北药学杂志,2016,31(5):497-500.
[15]钱卓真,汤水粉,罗方方,等.石斑鱼中阿维菌素类药物多残留测定及食用安全风险评估[J].食品科学,2017,38(22):309-316.
[2]杨二爽,李小莲,沈雁,等.高效液相色谱法测定乙酰氨基阿维菌素的含量[J].黑龙江畜牧兽医,2017(12):162-164.
[3]刘永涛,余琳雪,王桢月,等.改良的QuEChERS结合高效液相色谱-串联质谱同时测定水产品中7种阿维菌素类药物残留[J].色谱,2017,35(12):1276-1285.
[4]李建华,刘琴,周亚平,等.乙酰氨基阿维菌素对奶牛寄生虫治疗效果评价实验[J].中国畜牧兽医文摘,2018,34(2):254-241.
[5]都倩.多沙唑嗪的SPE-LC-MS/MS分析方法建立及其在大鼠体内代谢的研究[D].河石家庄北:河北医科大学,2017.
[6]丁杨,邓美荣,聂晶,等.固相萃取-高效液相色谱法测定乳制品中三聚氰胺的含量[J].中国卫生工程学,2016,15(1):41-45.
[7]冒玉娟,陈晓兰,赵丽.乙酰氨基阿维菌素在动物医学中的研究进展[J].畜牧与饲料科学,2013,34(1):86-89.
[8]Pollock J,Bedenice D,Jennings S H,et al.Pharmacokinetics of an extended-release formulation of eprinomectin in healthy adult alpacas and its use in alpacas confirmed with mange[J].J Vet pharmacol Ther,2017,40(2):192-199.
[9]Brique-Pellet C,Ravinet N,Quenet Y,et al.Pharmacokinetics and anthelmintic efficacy of injectable eprinomectin in goats[J].Vet Parasitol,2017,241(10):43-47.
[10]Lifschitz A,Nava S,Mangold A,et al.Eprinomectin accumulation in Rhipicephalus(Boophilus)microplus:Pharmacokinetic and efficacy assessment[J].Vet Parasitol,2016,215(2):11-16.
[11]高三玉,周芷锦,罗成江,等.高效液相色谱法测定牛奶中乙酰氨基阿维菌素的残留量[J].畜牧与饲料科学,2017,38(4):14-16.
[12]Wang Q,Zhao R,Cui Y,et al.Rapid and simple determination of sarafloxacin and difloxacin in beef by capillary electrophoresis coupled with solid-phase extraction[J].J Anal Methods Chem,2018,2018(8):19-36.
[13]Gokbulut C,Ozuicli M,Aksit D,et al.Comparative plasma and milk dispositions,faecal excretion and efficacy of per os ivermectin and pour-on eprinomectin in horses[J].J Vet Pharmacol Ther,2016,39(6):584-589.
[14]任丽君,郭玉娟,姚军,等.伊维菌素缓释注射液的制备工艺及在绵羊体内药代动力学研究[J].西北药学杂志,2016,31(5):497-500.
[15]钱卓真,汤水粉,罗方方,等.石斑鱼中阿维菌素类药物多残留测定及食用安全风险评估[J].食品科学,2017,38(22):309-316.