动物性食品中盐酸多西环素残留量荧光检测方法研究OACSTPCD
Optimization of fluorescence detection method for residues of doxycycline hydrochloride in animal-derived food
利用表面活性剂可以提高物质荧光强度这一原理以及固相萃取技术,建立荧光法检测动物性食品中盐酸多西环素残留量.讨论表面活性剂类型和加入量,反应温度、处理时间、加入顺序等条件对盐酸多西环素荧光强度的影响.设计了三因素三水平正交实验,优化样品前处理过程.选择Mcllvaine-Na2EDTA缓冲液作为提取剂,甲醇、乙酸乙酯(1∶9)混合液作为洗脱剂,涡旋萃取时间为 2 min.在 1 cm石英比色皿中,设定激发波长(λex)为 378 nm,发射波长(λem)为 438 nm,冰浴 30 min后扫描测定.在 7.14×10-4～5.71×10-2 mg/mL 时,盐酸多西环素的浓度和荧光强度线性关系较好(r=0.9995),检出限为 74.99 ng/mL,加标回收率为 79.93%～90.48%,相对标准偏差为 0.34%～0.73%.该方法可用于定性定量检测动物性食品中盐酸多西环素残留量.
In this study,fluorescence detection method for doxycycline hydrochloride residues in animal-derived food was established using the principle that surfactants can improve the fluorescence intensity of substances and solid-phase extraction technology.The effects of surfactant type and dosage,reaction temperature,treatment time and addition sequence on the fluorescence intensity of doxycycline hydrochloride were discussed.An orthogonal experiment with three factors and three levels was designed to optimize the pretreatment process of samples.Mcllvaine-Na2EDTA buffer was selected as extraction agent.The mixture of methanol and ethyl acetate(1:9)was selected as the eluent,and the extraction time was 2 min.The excitation wavelength(λex)was set to 378 nm and the emission wavelength(λem)to 438 nm in a 1 cm quartz colorimetric dish.When the concentration of doxycycline hydrochloride was within the range of 7.14×10-4～5.71×10-2 mg/mL,the linear relationship between the doxycycline hydrochloride concentration and fluorescence intensity was good,r=0.9995,with a detection limit of 74.99 ng/mL,the standard recovery was 79.93%～90.48%,and the relative standard deviation was 0.34%～0.73%.The method can be utilized for the qualitative and quantitative determination of doxycycline hydrochloride residues in animal-derived food.
李月秋;田进禄;徐天佑;王燕;张智;邸科前
河北大学基础医学院,保定 071000唐山市丰南区卫生监督所,丰南 063300新疆医科大学第一临床医学院,乌鲁木齐 830000
轻工业
盐酸多西环素吐温-20动物性食品固相萃取荧光分光光度法
doxycycline hydrochloridetween-20animal-derived foodsolid-phase extractionfluorescence spectrophotometry
《中国食品添加剂》 2024 (008)
20-27 / 8
河北省重点研发计划乡村振兴技术创新专项(22326605D);河北大学医学培育项目(2021B05)
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