高效液相色谱仪检测饲料中泰乐菌素方法的研究
摘要
泰乐菌素属大环内酯类抗生素,1999年,欧盟已禁止将泰乐菌素做为饲料添加剂使用,从2006年1月1日起,欧盟成员国全面禁止使用抗生素做为促生长剂,而在我国,泰乐菌素仍然属于饲料药物添加剂。
饲料中泰乐菌素的检测是由全国饲料标准技术委员会下达的制定国家标准项目。本试验旨在参考国内外现有先进检测技术基础上,兼顾我国饲料质检机构装备水平,采用高效液相色谱仪(HPLC)配备二极管阵列检测器进行方法摸索。建立了测定饲料中的泰乐菌素含量的高效液相色谱仪(HPLC)方法。
确定了用二氯甲烷提取饲料中的泰乐菌素(提取率最高,且干扰少)、用SPE小柱净化后上HPLC测定、检测波长为280 nm,流动相选用乙腈∶甲醇∶0.05 mol/L磷酸二氢铵=50∶35∶15、色谱柱选用symmtry shield RP18(250 mm×3.9 mm,4.5μm)。其回收率达到86.6%～99.8%,变异系数为0.2%～2.4%,在0.5～100μg/mL线性系数达到1。
本方法适于配合饲料、浓缩饲料和预混合饲料中泰乐菌素的检测。
本方法的最低检测限为1 mg/kg。
Tylosin belongs to the antibiotic of macrolides, and in1999, Tylosin has been forbidden as the additives in feeds by EU. From 1,Jan.2006, EU member states all forbidad using antibiotics as growth of,but in our country, the tylosin still belongs to feed additive drug.
National Feed Sdandards Technical Committee issued the item of detection for tylosin in feeds which is to establish the national standards.This experimentation would aim at consulting the advanced detection tecnology in existence at home and abroad and give attention to the equipment level of feed quality inspection agencies in our country, which adopted the array detector of HPLC with diode, compared the effect of distilling tylosin in samples with methanol, acetonitrile and dichloromethane, compared separating effects of different mobile phase and different chromatography columns. The result indicated with dichloromethane distilling its effect was best, the exdtract passed through filtrated, condensed, and was mensurated on HPLC. The detection wavelength is 280nm. With acetonitrile : methanol : 0.5mol NH4H2PO4/L = 50:35:15, selecting symmtry shield RP18 as chromatography column, its isolation attained demand. The recoveries was between 86.6~99.2%, the coefficient variation was 0.2~2.4%, the linear relationship was fine between 0.5μg/ml~ 100μg/ml, correlation coefficient attained 1, which indicated, under these conditions, the apparatus state was more steady. The methological loweast detection limits was 1㎎/㎏, and this detection method is both applicable to the premixes with higher content of tylosin and to mixed feeds with lowwer content of tylosin, at the same time, the method operating convenient, speediness, nicety, all accorded with the demond of feed detection.
饲料中泰乐菌素的检测是由全国饲料标准技术委员会下达的制定国家标准项目。本试验旨在参考国内外现有先进检测技术基础上,兼顾我国饲料质检机构装备水平,采用高效液相色谱仪(HPLC)配备二极管阵列检测器进行方法摸索。建立了测定饲料中的泰乐菌素含量的高效液相色谱仪(HPLC)方法。
确定了用二氯甲烷提取饲料中的泰乐菌素(提取率最高,且干扰少)、用SPE小柱净化后上HPLC测定、检测波长为280 nm,流动相选用乙腈∶甲醇∶0.05 mol/L磷酸二氢铵=50∶35∶15、色谱柱选用symmtry shield RP18(250 mm×3.9 mm,4.5μm)。其回收率达到86.6%～99.8%,变异系数为0.2%～2.4%,在0.5～100μg/mL线性系数达到1。
本方法适于配合饲料、浓缩饲料和预混合饲料中泰乐菌素的检测。
本方法的最低检测限为1 mg/kg。
Tylosin belongs to the antibiotic of macrolides, and in1999, Tylosin has been forbidden as the additives in feeds by EU. From 1,Jan.2006, EU member states all forbidad using antibiotics as growth of,but in our country, the tylosin still belongs to feed additive drug.
National Feed Sdandards Technical Committee issued the item of detection for tylosin in feeds which is to establish the national standards.This experimentation would aim at consulting the advanced detection tecnology in existence at home and abroad and give attention to the equipment level of feed quality inspection agencies in our country, which adopted the array detector of HPLC with diode, compared the effect of distilling tylosin in samples with methanol, acetonitrile and dichloromethane, compared separating effects of different mobile phase and different chromatography columns. The result indicated with dichloromethane distilling its effect was best, the exdtract passed through filtrated, condensed, and was mensurated on HPLC. The detection wavelength is 280nm. With acetonitrile : methanol : 0.5mol NH4H2PO4/L = 50:35:15, selecting symmtry shield RP18 as chromatography column, its isolation attained demand. The recoveries was between 86.6~99.2%, the coefficient variation was 0.2~2.4%, the linear relationship was fine between 0.5μg/ml~ 100μg/ml, correlation coefficient attained 1, which indicated, under these conditions, the apparatus state was more steady. The methological loweast detection limits was 1㎎/㎏, and this detection method is both applicable to the premixes with higher content of tylosin and to mixed feeds with lowwer content of tylosin, at the same time, the method operating convenient, speediness, nicety, all accorded with the demond of feed detection.
引文
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