元波,郭红燕袁,高又文,曾振灵.猪粪便和尿液中二甲氧苄啶的液相色谱串联质谱检测方法研究[J].广东农业科学,2013,40(17):101-103 |
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猪粪便和尿液中二甲氧苄啶的液相色谱串联质谱检测方法研究 |
Determination of diaveridine in pig faeces and urine by high performance liquid chromatographic tandem mass spectrometry |
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DOI: |
中文关键词: 二甲氧苄啶 猪 粪便 尿液 相串联质谱 |
英文关键词: diaveridine pig faeces urine LC-MS |
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中文摘要: |
试验旨在建立二甲氧苄啶在猪粪便和尿液中的液相色谱串联质谱检测方法。尿液经乙酸乙酯液液萃取,有机层经氮气吹干、35%乙腈水复溶后上机检测;粪便样品经酸乙酯提取,MCX 小柱净化后,洗脱液用氮气吹干,35%乙腈水复溶后上机检测。结果显示:猪粪便和尿液中二甲氧苄啶浓度分别在5~1 000 μg/kg 和10~1 000 μg/L范围内呈现良好的线性关系渊r>0.99冤,尿液尧粪便中二甲氧苄啶的定量限分别为10 μg/L 和5 μg/kg,尿液添加浓度为10、100、1 000 μg/L时的回收率分别为79.6%、84.3%、90.2%,粪便添加浓度为10、100、1 000 μg/kg 时的回收率分别为66.1%、65.1%、54.7%,批间、批内变异系数均小于14%,该方法定量限低,灵敏、准确,符合相关研究的要求。 |
英文摘要: |
A highperformance liquid chromatographic tandem mass spectrometry (LC-MS) method was presented for determination of diaveridine in pig faeces and urine. The urine sample was treated with ethyl acetate. The organic phase was evaporated and redissolved with acetonitrile /water (35:65); the faeces were extracted by ethyl acetate and purified with MCX solid phase extraction column, then the
eluant was evaporated and redissolved with acetonitrile /water (35:65).The result showed that the density of diaveridine in pig faeces and urine was in good linearity at the range of 5~1 000 μg/kg and 10~1 000 μg/L respectively (r>0.99).The limit of quantification (LOQ) in urine and faeces were 10 μg/L and 5 μg/kg respectively. The recovery was 79.6%, 84.3%,90.2% while blank swine urine spiked with diaveridine at 10, 100, 1 000 μg/L and the recovery was 66.1%, 65.1%, 54.7% while blank swine faeces spiked with diaveridine at 10, 100, 1 000 μg/kg respectively |
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