超高效液相色谱-串联质谱法检测牛可食性组织中氟佐隆残留

The Research of Fluazuron Residues in Cattle Edible Tissues by UPLC-MS/MS

建立了一种检测牛可食性组织中氟佐隆残留的超高效液相色谱-串联质谱法。牛肌肉、肝脏、肾脏和脂肪样品经90%乙腈溶液提取,高速离心去除蛋白质等杂质,EMR-Lipid柱净化。以0.1%甲酸乙腈溶液和0.1%甲酸水溶液为流动相,在C18色谱柱上分离。在电喷雾正离子(ESI+)模式下采用多反应监测模式(MRM)检测,基质匹配标准溶液外标法定量。结果表明:氟佐隆对牛肌肉在1~100 ng/mL浓度范围内,对牛肝脏、肾脏和脂肪在1~500 ng/mL浓度范围内均呈现良好的线性关系,决定系数(R2)均大于0.990;在4种牛可食性组织中氟佐隆的检测限均为5μg/kg,定量限均为10μg/kg。氟佐隆在牛肌肉10~400μg/kg、牛肝脏和牛肾脏10~1000μg/kg、牛脂肪10~14000μg/kg空白添加浓度范围内的回收率为72.0%~98.6%;批内与批间相对标准偏差均小于15%。该方法具有简便快捷、选择性好、定性准确,重复性好等特点,可以满足上述组织中氟佐隆残留检测的要求。

A UPLC-MS/MS method was established for the determination of fluazuron residues in 4 kinds of cattle edible tissues.Fluazuron was extracted from cattle muscle,liver,kidney and fat with acetonitrile solution(acetonitrile∶water=9∶1),and the protein was deposited by high speed centrifugation.Then the sample solutions were purified with EMR-Lipid column.The mobile phase were water(0.1%formic acid)and acetonitrile(0.1% formic acid),and the samples were separated by C18 column.Ionization was performed using an positive ion electrospray ionization(ESI+)applying the detection mode of multiple reaction monitoring(MRM).The method was quantified by matrix matched standard curves.Good linearities of the calibration curves were obtained with the range of 1~100 ng/mL in cattle muscle,and with the range of 1~500 ng/mL in cattle liver,kidney and fat,the coefficient of determination R2>0.990.The limit of detection of fluazuron was 5μg/kg,and the limit of quantification of fluazuron was 10μg/kg.The recoveries of fluazuron residues were 72.0%~98.6%,for cattle muscle at the concentrations of 10~400μg/kg,cattle liver and kidney at the concentrations of 10~1000μg/kg,and for cattle fat at the concentrations of 10~14000μg/kg.The intra-and inter-batch variation coefficients were both less than 15%.With good selectivity,accuracy and repeatability,the method can be applied for the determination of fluazuron residues in 4 kinds of cattle edible tissues.