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Study on the Sensitive Determination of Macrolides by Capillary Electrophoresis with Electrochemiluminescence Detection and Applications

Author: ShiYanMei
Tutor: LiuYanMing
School: Xinyang Normal University
Course: Analytical Chemistry
Keywords: Capillary Electrophoresis Electrochemiluminescence Macrolide antibiotics Bioanalytical Pharmacokinetics
CLC: R927
Type: Master's thesis
Year: 2010
Downloads: 76
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Abstract


Capillary electrophoresis (CE) is a kind of high-voltage electric field as the driving force to capillary separation channel, based on a variety of characteristics of the sample efficient separation and analysis technology, is the second gas chromatography (GC) and high performance liquid chromatography (HPLC ) after analysis of another major scientific progress. CE has the advantages of efficient, rapid and peak capacity, consumption of small sample and biological compatibility. However, due to the capillary inner diameter dimension (2-100μm), brought to the detection difficult, resulting in the detection sensitivity of the CE restricted. Therefore, to improve the detection sensitivity has become a very important research direction in the field of CE. Electrochemiluminescence (ECL) because of its high sensitivity, wide linear range, controllable reaction, reagent consumption, high efficiency of information analysis and reaction to appeal to a broad analysis of workers in many fields of interest. CE-ECL associated with high separation efficiency and high sensitivity characteristics. Can be used for the separation and determination of trace components in complex samples. In this paper, the CE-ECL, carried out the analysis and detection of some important macrolide antibiotics, main contents and innovations are as follows: 1. The first time to establish a CE-ECL sensitive detection of azithromycin (AZI), acetyl spiral mold the hormone (ACE), erythromycin (ERY) and josamycin (JOS). CE separation conditions and electrochemiluminescence detection conditions were studied systematically. Under optimized conditions, four kinds of macrolide analyte within 6 min to get a good separation. Of AZI, ACE, ERY and Jos limit of detection (LOD) were 1.2 × 10-9,7.1 × 10-9,3.9 × 10-8 and 9.5 × 10 8 mol / L. In the urine, AZI ACE, ERY, and JOS limit of quantitation (LOQ) were 8.2 × 10-8,2.5 × 10-7,8.9 × 10-7 and 1.2 x 10-6 mol / L. 4 analytes in urine and tablets of different levels spiked recoveries in the range of 85.0-104.0%. The new method was successfully used in human urine and tablets Determination. 2 internal standard CE-ECL combination of ionic liquids for the first time to create a sensitive determination of tilmicosin, Hu has erythromycin and clindamycin. CE separation conditions, the ECL detection conditions and the impact of the ionic liquid system optimization. Under optimized conditions, the three kinds of analyte and internal standard AZI 8 mmin baseline separation. After the ionic liquid BMIMBF4 as additives added to the electrophoresis buffer solution, effectively improve the separation efficiency and detection sensitivity. AZI as an internal standard, significantly improve the precision and accuracy of the method. Tilmicosin, Hu has erythromycin and clindamycin LOD, 3.4 × 10-9,2.3 × 10-8 and 1.3 × of 10-8mol / L. And the method used for the separation and analysis of the three analytes in human urine, milk and Drug. Tilmicosin, Hu erythromycin and clindamycin in the urine LOQ were 3.2 × 10-8,2.9 × 10-7 and 9.1 × 10 8 mol / L; LOQ in milk were The 5.5 × 10-8,3.2 x 10-7 and 2.1 x 10-7mol /. Different concentration levels in the urine, milk and drug recovery was in the range of 90.0% -104.7%. The new method was successfully applied to the separation and analysis of human urine, milk and pharmaceutical preparations. Establish a CE-ECL sensitive detection of the enoxacin and ofloxacin new method,. Conditions of separation and detection conditions were optimized. Under optimized conditions, enoxacin and ofloxacin 7min to achieve good separation. Using acetonitrile - water mixed solution of the solvent used as a sample, so that the separation efficiency and detection sensitivity are improved obviously. Enoxacin and ofloxacin LOD were 9.0 × 10-9 and 1.6 × 10 8 mol / L. Inter-day precision (RSD%) were less than 2.1% and 4.0%, respectively. The proposed method has been successfully applied to the determination of human urine, serum and eye drops enoxacin and ofloxacin. The under enoxacin and ofloxacin in the urine LOQ were 3.2 x 10-7 and 5.4 x 10 7 mol / L in serum LOQ were 4.1 x 10-7 and 6.9 x 10-7mol / L LOQ eye drops were 5.8 x 10-8 and 1.1 x 10-7mol / L. In the urine, serum, and eye drops recoveries were 94.0% -106.7%. The new method has been successfully used in the human body the ofloxacin urine pharmacokinetic study.

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