固相萃取-液相色谱串联质谱法测定猪尿中的巴氯芬 |
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引用本文: | 夏 骏. 固相萃取-液相色谱串联质谱法测定猪尿中的巴氯芬[J]. 中国兽药杂志, 2013, 47(5): 32-35 |
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作者姓名: | 夏 骏 |
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作者单位: | 江西省兽药饲料监察所,江西 南昌 邮编 |
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摘 要: | 为了建立用固相萃取-液相色谱串联质谱法测定动物尿液中巴氯芬药物残留的检测方法,试验采用叔丁醇-叔丁基甲醚对猪尿样品进行提取,提取液经混合型阳离子固相萃取小柱(MCX)净化、富集后,以液相色谱串联质谱测定,外标法定量。结果表明,该方法检出限为0.2 ng/mL,定量限为0.8 ng/mL,巴氯芬在0.8~20 ng/mL的添加浓度范围内线性良好,线性相关系数大于0.9997,在低、中、高(0.8、1.6、5.0 ng/mL)三个浓度的添加水平回收率在80%~120%之间,批内、批间精密度均小于10%。该方法灵敏度高,定性、定量准确,可用于猪尿中巴氯芬药物残留的定性、定量检测。
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关 键 词: | 巴氯芬;猪尿;液相色谱-串联质谱法;残留 |
收稿时间: | 2013-02-22 |
修稿时间: | 2013-04-05 |
Determination of Baclofen in Pig Urine by High-Performance Liquid Chromatograph-Tandem Mass Spectrometry |
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Affiliation: | Jiangxi Province Institute of Veterinary Drug and Feed Control |
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Abstract: | A simple and sensitive LC-MS/MS method for determination of baclofen in pig urine was developed. The sample was extracted by the mixture of tert-butanol and tert-butyl methyl ether, and purified by MCX cartridges. The analyte was determined by LC-MS/MS with extermal standard for quantification. The limit of detection and limit of quantity were found to be 0.2 ng/mL and 0.8 ng/mL, respectively. The standard curve of baclofen within the range of 0.8 to 20 ng/mL was in good linearity, the correlation coefficients were greater than 0.9995, the recoveries ranged from 80% to 120%(0.8,1.6,5.0 ng/mL), and intra- and inter-batch variation coefficients were lower than 10% for low, middle and high concentrations. |
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Keywords: | baclofen pig urine LC-MS/MS residue |
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