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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
王亦琳,尹晖,叶妮,孙雷,王鹤佳
0
(中国兽医药品监察所)
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。
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
DOI:
投稿时间:2020-07-01修订日期:2020-08-20
基金项目:
Research of Pirlimycin Residues in Cattle Edible Tissues by Liq The uid Chromatography-Quadruple/Linear Ion Trap Mass Spectrometry
(China Institute of Veterinary Drug Control)
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.
Key words:  LC-Q-trap MS  cattle edible tissues  pirlimycin  residues analysis

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