十二烷基硫酸钠胶束相萃取生物碱的进一步色谱测定

IF 0.7 Q4 CHEMISTRY, ANALYTICAL Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI:10.17721/moca.2023.81-86
V.S. Starova, S.A. Kulichenko
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引用次数: 0

摘要

研究了部分生物碱的疏水性(log P)、结构(PSA)和水解性能(pKa)等主要参数对其在十二烷基硫酸钠(SDS-NaCl-H2Sal)改性胶束萃取体系中的分布的影响。所提出的预后回归D= 941 - 4.09∙PSA - 27.3∙log P - 44.5∙рКа指标令人满意(r方99.9,f比242,标准误差7.19,平均绝对误差2.38)。该回归预测生物碱分布的准确度与提取参数测量的准确度具有良好的相关性。对诺佛卡因的预测D值为257 (R = 93%),实验发现D值为202 (R = 91%)。利多卡因的预测D值与实验D值基本一致,分别为386 (R = 95%)和380 (R = 95%)。带正电的亲水性(logP <0)有机碱进入SDS胶束相。采用改性胶束SDS相对尿液中阳离子形态(pH=2)的罂粟碱进行预富集的混合高效液相色谱技术具有足够的灵敏度和准确性(DL= 0.01 μg/ml, Sr≤0.08,R >99%, k = 10)。只有生物碱具有对数P >1.4由于水杨酸和生物碱的色谱峰不能分离,所以可以用该技术进行测定。
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Extraction of Alkaloids by the Micellar Phase of Sodium Dodecyl Sulfate for their Further Chromatographic Determination
The influence of the main parameters of hydrophobicity (log P), structure (PSA), and protolytic properties (pKa) of some alkaloids on their distribution into modified micellar extraction system based on sodium dodecyl sulfate (SDS-NaCl-H2Sal) was established. The proposed prognostic regression D= 941 – 4.09∙PSA – 27.3∙log P – 44.5∙рКа is characterized by satisfactory indexes (R-squared 99.9, F-ratio 242, standard error 7.19, mean absolute error 2.38). The accuracy of the alkaloid distribution prediction by this regression is well correlated with accuracy of the measurement of the extraction parameters. The predicted D value for novocaine is 257 (R = 93 %), and the experimentally found D value is 202 (R = 91 %). For lidocaine, the predicted and experimental D values are practically the same and equal 386 (R = 95 %) and 380 (R = 95 %), respectively. The possibility of quantitative extraction of positively charged hydrophilic (logP < 0) organic bases into the micellar phase of SDS is shown. The developed hybrid HPLC technique for determining papaverine in urine with its cationic form (pH=2) preconcentration by modified micellar SDS phase is characterized by sufficient sensitivity and accuracy (DL= 0.01 μg/ml, Sr ≤ 0.08, R > 99 %, K = 10). Only alkaloids with log P > 1.4 can be determined by this technique because otherwise, the chromatographic peaks of salicylic acid and alkaloid cannot separate.
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来源期刊
CiteScore
1.00
自引率
14.30%
发文量
12
期刊介绍: The journal "Methods and objects of chemical analysis" is peer-review journal and publishes original articles of theoretical and experimental analysis on topical issues and bio-analytical chemistry, chemical and pharmaceutical analysis, as well as chemical metrology. Submitted works shall cover the results of completed studies and shall make scientific contributions to the relevant area of expertise. The journal publishes review articles, research articles and articles related to latest developments of analytical instrumentations.
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