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

关键词:  超高效液相色谱-串联质谱  牛可食性组织  氟佐隆  残留

Key words:  UPLC-MS/MS  cattle edible tissues  fluazuron  residues

摘要:

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-串联质谱方法。牛肌肉、肝脏、肾脏和脂肪样品经90%乙腈水溶液提取，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5 μg/kg，定量限均为10 μg/kg。氟佐隆在牛肌肉10～400 μg/kg、牛肝脏和牛肾脏10～1000 μg/kg、牛脂肪10～14000 μg/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。

Abstract:

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 ofdeterminationcorrelation coefficient R2＞0.990. The limit of detection of fluazuron was 5 μg/kg, and the limit of quantification of fluazuron was 10 μg/kg. The recoveries of fluazuron residues were 72.0%～98.6%, for cattle muscle at the concentrations of 10～400 μg/kg, cattle liver and kidney at the concentrations of 10～1000 μg/kg, and for cattle fat at the concentrations of 10～14000 μg/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.