Determination of Picogram-Levels of Acetylspiramycin in Human Urine and Serum by Flow Injection Chemiluminescence

A sensitive chemiluminescence method for the determination of acetylspiramycin is presented. It is based on the greatly enhancive effect of acetylspiramycin on the chemiluminescence reaction between luminol and hydrogen peroxide in the flow system. The increase in chemiluminescence intensity was linearly proportional to the acetylspiramycin concentration in the range from 10pg·mL^–1 to 2.0ng·mL^–1 (r²=0.9979). The detection limit was 3pg·mL^–1 (3). At a flow rate of 2.0mL·min^–1, the process of determination, including sampling and washing, could be performed in 0.5 min, and the relative standard deviations of seven replicates are less than 5.0%. The proposed method was applied successfully to the determination of acetylspiramycin in pharmaceutical preparations, human urine and serum without pre-treatment. It was found that the excretive ratio of acetylspiramycin reached its maximum 2.0 hours after having been administered orally, and the excretive ratio in 12.0 hours was 8.4.     

Impurity profiling of acetylspiramycin by liquid chromatography–ion trap mass spectrometry

Investigation of acetylspiramycin (ASPM) and its related substances was carried out using a reversed-phase liquid chromatography/tandem mass spectrometry method. The identification of impurities in the ASPM complex was performed with a quadrupole ion trap mass spectrometer, with an electrospray ionization (ESI) source in the positive ion mode which provides MSⁿ capability. A total of 83 compounds were characterized in commercial samples, among which 31 impurities that had never been reported and 31 partially characterized impurities were deduced using the collision-induced dissociation (CID) spectra of major ASPM components as templates. Most of the major impurities arise from the starting materials and the synthesis process. This work provides very useful information for quality control of ASPM and evaluation of its synthesis process.     

硫酸颜色反应用于乙酰螺旋霉素的同步荧光法测定

提出了硫酸颜色反应用于乙酰螺旋霉素的荧光法测定的新方法。乙酰螺旋霉素本身为弱荧光物质，与沈硫酸反应后生成强荧光物质。以Δλ＝１６ｎｍ进行同步扫描，所得的同步荧光光谱在４９０ｎｍ处的荧光强度与乙酰螺旋霉素的浓度在２０μｇ／Ｌ￣７ｍｇ／Ｌ的东南人线性关系良好。方法的检测限为７μｇ／Ｌ。本法可直接用于尿液中乙酰螺旋霉素的定量分析，回收率为８３．３％￣８８．７％。     

药物分子在玻碳电极上的电分析化学研究——Ⅳ.乙酰螺旋霉素的伏安测定

本文对乙酰螺旋霉素在GCE上的伏安行为进行了研究,发现在磷酸盐缓冲溶液(pH=7.87)中,於十0.85V(vs.Ag/AgCl)左右产生一良好的阳极氧化伏安峰.浓度在0.5～100μg/mL之间与峰电流呈线性关系,分析了制剂中乙酰螺旋霉素的含量,相对标准偏差为4.5%,平均回收率为101%.经循环伏安法验证,电极反应为不可逆反应.     

乙酰螺旋霉素的间接光度法测定

本文建立了一种乙酰螺旋霉素的新的分析方法，乙酰螺旋霉素在盐酸、磷酸混合液中显棕色，该溶液在470nm处有最大吸收，可用于乙酰螺旋霉素的间接光度法测定。其其线性范围是2.0-50.0mg/mL，相关系数是0.9995，回归方程是y=3.56×10^-3＋1.025C。本法用于乙酰螺旋霉素的实际样品测定，结果令人满意。     

乙酰螺旋霉素的一阶导数光谱法测定

在０－２５μｇ／ｍＬ范围内，国酰螺旋素一阶导数光谱在２２０－２５０ｎｍ之间的峰谷振幅Ｄ与浓度呈现良好的线性关系，基于此建立了乙酰螺旋霉素的分析方法。该法回归方程为Ｃ＝３．０９Ｄ－０．２４７，相关系数为０．９９９６，直接用于乙酰螺旋霉素片的测定，结果令人满意。     

Artificial neural networks for non-destructive determination of acetylspiramycin powder by short-wavelength NIR spectroscopy

The present study has aimed at providing new insight into short-wavelength near-infrared (SW-NIR) spectroscopy (780–1100 nm) for non-destructive quantitative analysis of acetylspiramycin (macrolide antibiotics) powder by using artificial neural networks (ANNs). Presently, it was shown the third vibrational overtone of the CH stretching band can be used to quantitatively determine constituents in pharmaceutical. The third overtone referred to as the SW-NIR region ranges from 780 nm to 1100 nm. In this paper, 156 experimental samples of acetylspiramycin powder were analyzed using ANNs in the 780–1100 nm region of SW-NIR spectra. Four different pretreated methods (first-derivative, second-derivative, standard normal variate (SNV) and multiplicative scatter correction (MSC)) were applied to three sets of SW-NIR spectra of powder samples. The results presented here demonstrate that the SW-NIR region is promising for the fast and reliable determination of major component in pharmaceutical analysis. Degree of approximation as an evaluation criterion of the network was employed, which proved the accuracy of the predicted results.     

乙酸螺旋霉素的单扫示波极谱研究

本文报道了一种新的、灵敏的乙酰螺旋霉素测定法——二阶导数单扫示波极谱分析法.在 0.05 mol/L NaOH介质中,乙酰螺旋霉素有一灵敏的还原峰E_p~″=-1.52(vs.SCE),二阶导数峰电流i_p~″与浓度在 5.0~90μg/mL范围内存在线性关系,RSD=3.6%(n=6),检测限为 2.0μg/mL(S/N=2.5);经多种实验证明其电极过程为含弱吸附的不可逆扩散控制过程,电子转移数为2.此外还研究了人体内共存微量物质对i_p~″的影响;该法用于乙酰螺旋霉素药片含量分析,结果令人满意.     

乙酰螺旋霉素活性成分的分析

乙酰螺旋霉素是一种含有多个活性成分的抗生素药物，本文首先用电喷雾质谱法测定了混合物的组成，然后采用高效液相色谱和微乳毛细管电泳法分离了其中的活性成分，用液相色谱－质谱联用技术鉴定了液相色谱的流出峰。