煤基碳量子点荧光猝灭法测定注射液和牛奶样品中卡那霉素  

Fluorimetric Determination of Kanamycin in Injections and Milk Samples by Quenching of Fluorescence of Carbon Quantum Dots by Kanamycin

作　　者：毛永强[1] 张喆双娇 孙一鑫 李娜[1] MAO Yongqiang;ZHANG Zheshuangjiao;SUN Yixin;LI Na(College of Science,Liaoning Technical University,Fujcin 123000,China)

机构地区：[1]辽宁工程技术大学理学院

出　　处：《理化检验（化学分册）》2019年第12期1401-1405,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：辽宁省自然科学基金(201602358);校第六批生产技术问题创新研究基金(20160087T);辽宁省大学生创新创业训练计划资助项目(201810147242,201710147094)

摘　　要：制备了煤基碳量子点(CQDs),此纳米材料具有较高的荧光强度,在激发波长(λex)为370nm时,其发射波长(λem)为495nm。卡那霉素(KANA)对CQDs的荧光具有猝灭效应,并测得其荧光强度的猝灭程序与KANA的浓度在5.0~140.0μmol·L-1之间呈线性关系,KANA的检出限(3s/k)为1.0μmol·L-1。根据进一步试验提出了KANA注射液及牛奶中KANA含量的荧光猝灭测定法。CQDs与KANA反应的最佳条件为:①反应介质为pH 7.5三(羟甲基)氨基甲烷(Tris-HCl)缓冲溶液;②CQDs溶液的加入量为0.5mL;③反应时间为10min。两种样品溶液的制备方法如下:①取KANA注射液5支,混匀后分取0.1mL,加水定容至100.0mL,经滤膜过滤,取滤液作为测定溶液;②取牛奶10.0g,加无水乙醇定容至50.0mL,静置30min后离心,取其上清液为测定溶液。测定时取测定液适量,加入Tris-HCl缓冲溶液和CQDs溶液各0.5mL,加水至5.0mL,按上述条件测定其荧光强度(F),同时测定空白溶液的荧光强度(F0)。经回收试验,测得其回收率在97.0%~104%之间,测定值的相对标准偏差(n=6)在1.2%~2.6%之间。经用高效液相色谱法作比对,两种方法所测得的结果相符。测得KANA注射液样品的KANA测定值为99.6g·L-1,与其标示值(100g·L-1)相符。Carbon quantum dots(CQDs),a kind of nanomaterial possessing high fluorescence intensity,were prepared from coal powdow.At the excitation wavelength(λex)of 370 nm,CQDs showed its emission wavelength(λem)of 495 nm.Kanamycin(KANA)showed quenching effect on the fluorescence of CQDs,and the magnitude of the decrease of fluorescence intensity of CQDs was found to keep a linear relationship with concentration of KANA in the range of 5.0 to 140.0μmol·L-1,with detection limit(3 s/k)of KANA 1.0μmol·L-1.Further testings were made for applying this fluorescence quenching reaction to determination of KANA in its injections and in milk samples.The optimum reaction conditions were given as follows:① the reaction medium chosen was pH 7.5 tri(hydroxymethyl)aminomethane(Tris-HCl)buffer solution;② amount of CQDs added was 0.5 mL;and ③reaction time was 10 min.Preparation of sample solutions was done as follows:①for KANA injection sample,5 injections were taken and mixed thoroughly,an aliquot of 0.1 mL was taken and diluted to 100.0 mL with water.After filtering through filtering membrane,the filtrate was used for determination;②for milk samples,10.0 g of the sample were taken and diksted to 50.0 mL with absolute alcohol.After staying for 30 min,the mixed solution was centrifuged,and the surpernatant was used for determination.An appropriate amount of the sample solution was taken,and 0.5 mL each of the Tris-HCl buffer solution and ths CQDs were added to the sample solution,and the volume was made up to 5.0 mL with water.Fluorescence intensity(F)of the solution was measured under the condition given above,and fluorescence intensity(F0)of blank solution was measured simultaneously.Values of recovery found by recovery test were found in the range of 97.0%to 104%,and RSDs(n=6)found were ranged between 1.2% and 2.6%.Samples were analyzed by the present method and checked by HPLC determination,results obtained by the 2 methods were found in good conformity.Result of KANA found in injection sample(99.6 g·L-1)was in consist

关 键 词：碳量子点 卡那霉素 荧光猝灭 注射液 牛奶 

分 类 号：O657.31[理学—分析化学]