猪肉中4种硝基呋喃类药物的纳米纤维固相萃取快速前处理及检测方法的建立

Rapid pretreatment and determination of four nitrofuran drugs in pork by nanofiber solid phase extraction

建立纳米纤维固相萃取-高效液相色谱-紫外(PFSPE-HPLC-UV)检测猪肉中呋喃妥因(AHD)、呋喃西林(SEM)、呋喃唑酮(AOZ)、呋喃它酮(AMOZ)的检测方法.样品经过粉碎均质、超声、冷冻离心、稀释,取500μL柱上液过聚吡咯纳米纤维固相萃取柱,用100μL的8 mol/L硫酸-甲醇(15∶85)混合溶液洗脱,洗脱液混匀,以C18色谱柱分离目标物.4种目标物在浓度范围为10~1000 ng/mL时,线性关系良好;方法检出限为2.07~7.17 ng/mL,定量限为6.91~23.90 ng/mL.该方法的样品前处理方法集分离、净化、富集于一体,操作简便、快速,易于推广,且较传统的实验方法简单、精确性好、低耗高效,能够用于猪肉中硝基呋喃类的测定.

A nanofiber solid-phase extraction-high performance liquid chromatography-ultraviolet(PFSPE-HPLC-UV)method was established for the detection of nitrofurantoin(AHD),nitrofurazone(SEM),furazolidone(AOZ)and nitrofuranone(AMOZ)in pork.After being pulverized homogenized,sonicated,freezed,centrifuged,and diluted,500μL supernatant from the column was passed through a polypyrrole nanofiber solid-phase extraction column,and then 100μL 15%8 mol/L H_(2)SO_(4) mixed methanol solution was used as elute.The target compounds were separated by C18 chromatographic column.The four target compounds showed good linearity from 10 to1000 ng/mL;the detection limit of the method was 2.07~7.17 ng/mL,and the quantification limit was 6.91~23.90 ng/mL.The sample pretreatment method was formed by separation,purification and enrichment,easy to operate and popularize.Compared with traditional experimental methods,it is simple,accurate,low-consumption and high-efficiency,and can be used for the detection of nitrofurans in pork.