共振光散射光谱法和可见分光光度法测定酒石酸泰乐菌素的含量  

Determination of Tylosin Tartrate by Resonance Light Scattering Spectrometry and Visible Spectrophotometry

作　　者：袁莉 刘毅 储文 袁嘉怡 马卫兴 YUAN Li;LIU Yi;CHU Wen;YUAN Jiayi;MA Weixing(School of Pharmacy,Jiangsu Ocean University,Lianyungang 222005,China;School of Biomedical Industry,Jiangsu Ocean University,Lianyungang 222005,China;Key Laboratory of Marine Drug Screening of Jiangsu Province,Lianyungang 222005,China)

机构地区：[1]江苏海洋大学药学院,连云港222005 [2]江苏海洋大学生物医药产业学院,连云港222005 [3]江苏省海洋药物筛选重点实验室,连云港222005

出　　处：《理化检验（化学分册）》2024年第4期358-364,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江苏省品牌专业二期工程“省特色专业-药物制剂”(编号65);2021年江苏省首批一流本科课程“线下一流课程-药物分析”(序号104)等项目的大力支持。

摘　　要：将注射用酒石酸泰乐菌素样品稀释一定倍数后,分取1.20 mL样品稀释液、1.25 mL pH 3.0 Clark-Lubs(克拉克-鲁布斯)缓冲溶液和1.25 mL 1×10^(-4)mol·L^(-1)虎红溶液,室温反应20 min,用水稀释至10 mL。在315 nm处分别测量空白溶液(I_(0))及样品溶液(I)的共振光散射强度,计算共振光散射强度差值ΔI=I-I_(0)。分取1.00 mL样品稀释液、0.75 mL pH 3.4 Clark-Lubs缓冲溶液和2.50 mL 5×10^(-4)mol·L^(-1)虎红溶液,室温反应30 min,用水稀释至10 mL。以水为参比,在564 nm处测量空白溶液(A_(0))和样品溶液(A)的吸光度,计算吸光度差值ΔA=A-A_(0)。结果显示:酒石酸泰乐菌素的质量浓度分别在0.3~1.2 mg·L^(-1)内和ΔI呈线性关系,在4.0~48.0 mg·L^(-1)内和ΔA呈线性关系。2种方法的检出限分别为0.022 mg·L^(-1)和0.107 mg·L^(-1),回收率分别为99.0%~101%和98.2%~101%,测定值的RSD均小于1.0%。推断了2种方法的反应机理,ΔI和ΔA随酒石酸泰乐菌素质量浓度增加而增大的现象均和形成了离子缔合型超分子聚集体有关,形成的离子缔合型超分子聚集体中酒石酸泰乐菌素和虎红的物质的量比分别为1:6和1:24。The sample of tylosin tartrate injection was diluted a certain degree,and then an aliquot(1.20 mL)of sample diluent was taken and mixed with 1.25 mL of pH 3.0 Clark-Lubs buffer solution and 1.25 mL 1×10^(-4)mol·L^(-1)tiger red solution.After reacting at room temperature for 20 min,the solution was diluted to 10 mL by water.The resonance light scattering intensities of the blank solution(I_(0))and the determination solution(I)were measured at 315 nm,respectively.The difference(ΔI)in resonance light scattering intensities was calculated by I-I_(0).An aliquot(1.00 mL)of sample diluent was taken,and mixed with 0.75 mL of pH 3.4 Clark-Lubs buffer solution and 2.50 mL of 5×10^(-4)mol·L^(-1)tiger red solution.After reacting at room temperature for 30 min,the solution was diluted to 10 mL by water.The absorbance of the blank solution(A_(0))and the sample solution(A)was measured at 564 nm using water as a reference,and the absorbance difference(ΔA)was calculated by A-A_(0).It was shown that the mass concentration of tylosin tartrate showed a linear relationship withΔI in the range of 0.3-1.2 mg·L^(-1),and a linear relationship withΔA in the range of 4.0-48.0 mg·L^(-1).For the 2 methods,detection limits were 0.022 mg·L^(-1)and 0.107 mg·L^(-1),recoveries were 99.0%-101%and 98.2%-101%,and RSDs of the determined values were less than 1.0%.The reaction mechanisms of the 2 methods were inferred,and phenomenon aboutΔI andΔA increasing with the increase of the mass concentration of tylosin tartrate was related to the formation of ion associated supramolecular aggregates.The molar ratios of tylosin tartrate to tiger red in the ion associated supramolecular aggregates were 1:6 and 1:24,respectively.

关 键 词：酒石酸泰乐菌素 虎红 离子缔合型超分子聚集体 共振光散射光谱法 可见分光光度法 

分 类 号：R917[医药卫生—药物分析学] O657.3[医药卫生—药学]