在線固相萃取結(jié)合高效液相色譜—電噴霧式檢測器測定雞糞中紅霉素殘留

周茜等

摘 要 將在線固相萃取（online SPE）與高效液相色譜（HPLC）通用型電噴霧檢測器（CAD）結(jié)合，建立了集約養(yǎng)殖業(yè)常用抗生素紅霉素的分析方法。5.0 g 雞糞樣品與硅藻土混合后，置于34 mL萃取池中，以熱水為萃取劑，在70 ℃、10.4 MPa條件下，用快速溶劑萃取儀提取樣品中的紅霉素。利用雙三元液相色譜儀，采用在線富集進(jìn)樣方式，經(jīng)Acclaim 120 C18色譜柱，以乙腈0.1%甲酸溶液為流動(dòng)相分離后，用CAD進(jìn)行檢測。紅霉素在21～2000 μg/kg范圍內(nèi)線性關(guān)系良好（r≥0.99），檢出限為6.3 μg/kg，加標(biāo)回收率為79.2%～87.5%。

3.4 樣品加標(biāo)回收率

選用不含紅霉素的雞糞為測試對(duì)象，在50， 100和150 μg/kg加標(biāo)濃度下，測定樣品的抗生素加標(biāo)回收率分別為79.2%， 82.6%和87.5%。

3.5 實(shí)際樣品分析

將從集約養(yǎng)雞場抽取的10個(gè)雞糞樣品按本方法進(jìn)行處理和檢驗(yàn)，結(jié)果表明，雞糞樣品中的紅霉素譜圖見圖2。有6個(gè)樣品有紅霉素檢出，其中最高含量為1 mg/kg，最低含量為200 μg/kg，說明雞糞中含有不同程度的紅霉素殘留。

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Determination of Erythrocin in Chicken Manure by High Performance

Liquid ChromatographyCoronaCharged Aerosol Detection

Coupled with Online Solid Phase Extraction

ZHOU Qian1， CHEN ManTang1， ZHU LiHua1， DING Yao Bin2

1（College of Chemistry and Chemical Engineering， Huazhong University of Science and Technology， Wuhan 430074， China）

2（College of Chemistry and Material Science， SouthCentral University for Nationalities， Wuhan 430074， China）

Abstract A novel HPLCCAD method coupled with online solid phase extraction （SPE） for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite， 5.0 g manure sample was put into the cell and extracted with hot water at 70 ℃ and 10.3 MPa. An online SPE methodology was applied to pretreat the sample， and the sample was seperated on an Acclaim 120 C18 column and analyzed by corona CAD detector using acetonitrile and 0.1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6.3 μg/kg. The average recoveries were 79.2%-87.5%.

Keywords High performance liquid chromatography； Coronacharged aerosol detector； Online solid phase extraction； Erythrocin； Accelerated solvent extraction

（Received 25 August 2014； accepted 8 October 2014）

This work was partially supports by the National High Technology Research and Development Program of China （No. 2012AA06A304）

Abstract A novel HPLCCAD method coupled with online solid phase extraction （SPE） for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite， 5.0 g manure sample was put into the cell and extracted with hot water at 70 ℃ and 10.3 MPa. An online SPE methodology was applied to pretreat the sample， and the sample was seperated on an Acclaim 120 C18 column and analyzed by corona CAD detector using acetonitrile and 0.1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6.3 μg/kg. The average recoveries were 79.2%-87.5%.

Keywords High performance liquid chromatography； Coronacharged aerosol detector； Online solid phase extraction； Erythrocin； Accelerated solvent extraction

（Received 25 August 2014； accepted 8 October 2014）

This work was partially supports by the National High Technology Research and Development Program of China （No. 2012AA06A304）

Abstract A novel HPLCCAD method coupled with online solid phase extraction （SPE） for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite， 5.0 g manure sample was put into the cell and extracted with hot water at 70 ℃ and 10.3 MPa. An online SPE methodology was applied to pretreat the sample， and the sample was seperated on an Acclaim 120 C18 column and analyzed by corona CAD detector using acetonitrile and 0.1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6.3 μg/kg. The average recoveries were 79.2%-87.5%.

Keywords High performance liquid chromatography； Coronacharged aerosol detector； Online solid phase extraction； Erythrocin； Accelerated solvent extraction

（Received 25 August 2014； accepted 8 October 2014）

This work was partially supports by the National High Technology Research and Development Program of China （No. 2012AA06A304）