液相色谱-三重四级杆/线性离子阱复合质谱技术检测牛可食性组织中吡利霉素的残留

Research of Pirlimycin Residues in Cattle Edible Tissues by Liq The uid Chromatography-Quadruple/Linear Ion Trap Mass Spectrometry

关键词:  液相色谱-三重四级杆/线性离子阱  牛可食性组织  吡利霉素  残留检测

Key words:  LC-Q-trap MS  cattle edible tissues  pirlimycin  residues analysis

摘要:

建立了一种可准确定性定量检测4种牛可食性组织中吡利霉素残留的液相色谱-三重四级杆/线性离子阱（LC-Q-trap MS）复合质谱分析技术。牛肌肉、脂肪、肾脏和肝脏样品经5%甲酸乙腈提取，captiva EMR-Lipid柱净化。以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相，经Kinetex F5 色谱柱分离后，用多反应监测联合信息依赖性采集与增强子离子扫描（MRM-IDA-EPI）模式检测，基质匹配标准溶液校正，外标法定量。结果表明：吡利霉素于牛肌肉和脂肪中在1～100 ng/mL的浓度范围内，于牛肾脏和肝脏中在1～400 ng/mL浓度范围内均呈现良好的线性关系，关系数（R2）均大于0.990；在4种空白组织中吡利霉素的检测限均为5 μg/kg，定量限均为1相0 μg/kg。吡利霉素在牛肌肉和牛脂肪10～200 μg/kg、牛肾脏10～800 μg/kg，以及牛肝脏10～2000 μg/kg添加浓度范围内的回收率范围在60.2%～101%之间；批内与批间相对标准偏差均小于13%。该方法具有简便快速、灵敏度高、定性准确，重复性好等特点，可以满足上述组织中吡利霉素残留检测的要求。

Abstract:

A liquid chromatography-quadruple/linear ion trap mass spectrometry (LC-Q-trap MS） method with good accuracy was established for the determination of pirlimycin residues in 4 kinds of cattle edible tissues. Pirlimycin was extracted from cattle muscle, fat, kidney and liver with acetonitrile (5% formic acid). Then the sample solutions were purified with captiva EMR-Lipid column. The mobile phase were water (0.1% formic acid) and acetonitrile(0.1% formic acid), and the samples were separated by Kinetex F5 column. LC-Q-trap MS analysis was performed by positive ion electrospray ionization (ESI+) applying the detection mode of MRM-IDA-EPI. The method was quantified by matrix matching standard curves. Good linearities of the calibration curves were obtained with the range of 1~100 ng/mL in cattle muscle and fat, and with the range of 1~400 ng/mL in cattle kidney and liver, the correlation coefficient R2＞0.990. The limit of detection of pirlimycin was 5 μg/kg, and the limit of quantification of pirlimycin was 10 μg/kg. The recoveries of pirlimycin residues were 60.2%～101%, for cattle muscle and fat at the concentrations of 10～200 μg/kg, cattle kidney at the concentrations of 10～800 μg/kg, and for cattle liver at the concentrations of 10～2000 μg/kg. The intra-batch and inter-batch variation coefficients were both less than 13%. With high sensitivity, good accuracy and repeatability, the method can be applied for the determination of pirlimycin residues in 4 kinds of cattle edible tissues.