Abstract

A simple in-house UV-photolysis setup was utilized in this work as a sample pre-treatment for the decomposition of fluorinated pharmaceutical drugs and oral hygienic products. The sample decomposition process involved the passage of very dilute solutions of HClO₄ and H₂O₂ as a reagent mixture in dynamic mode through a PTFE coil wound over a UV lamp for irradiation followed by the quantification of fluoride by spectrophotometry based on bleaching of Zr−xylenol orange complex by fluoride. The optimization involved the study of the following critical parameters affecting the UV-photolytic decomposition (UVPD): concentration of the extractant mixture (HClO₄ and H₂O₂), sample flow rate and length of the PTFE reaction coil to get a quantitative recovery of fluoride. The methodology was optimized by using three bulk drugs, namely, afatinib, dolutegravir and fluphenazine, chosen as representatives of three diverse compounds. Using the experimental conditions established during optimization, the developed method (5 mL of mixture of 0.4% (v/v) HClO₄ and 0.2% (v/v) H₂O₂, a sample flow rate of 2.5 mL/min and a 1.5 m coil length), it was possible to completely converse the covalently bound fluorine to free fluoride ion for its subsequent determination by spectrophotometry. Quantitative recovery (>98%) of fluorine in all the test samples with a detection limit of 0.18 µg/g was achieved. Accuracy was evaluated by comparison of results obtained by the present UVPD method with the values of formula weights of the compounds. No statistical difference was observed between the results based on the paired t-test at a 95% confidence level. The optimized UVPD approach was subsequently applied to various pharmaceutical drugs and oral hygienic products (toothpaste and mouthwash) of a few leading brands purchased from the local market.

中文翻译：

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用于分解含氟药物和卫生产品以及分光光度法测定氟化物的紫外光解装置

摘要

在这项工作中，一个简单的内部紫外线光解装置被用作分解氟化药物和口腔卫生产品的样品预处理。样品分解过程包括 HClO ₄和 H ₂ O ₂作为试剂混合物的非常稀的溶液以动态模式通过缠绕在紫外线灯上的 PTFE 线圈进行照射，然后通过基于 Zr 漂白的分光光度法定量氟化物-二甲苯酚橙与氟化物形成络合物。优化涉及研究以下影响 UV 光解分解 ( UVPD ) 的关键参数：萃取剂混合物的浓度（HClO ₄和 H ₂ O ₂)、样品流速和 PTFE 反应盘管的长度，以获得氟化物的定量回收率。该方法通过使用三种原料药进行优化，即阿法替尼、多替拉韦和氟奋乃静，选择作为三种不同化合物的代表。使用优化过程中建立的实验条件，开发的方法（5 mL 0.4% (v/v) HClO ₄和 0.2% (v/v) H ₂ O ₂的混合物，样品流速为 2.5 mL/min 和 1.5 m 线圈长度），可以将共价结合的氟完全转化为游离氟离子，以便随后通过分光光度法进行测定。所有测试样品中氟的定量回收率 (>98%) 均达到了 0.18 µg/g 的检测限。通过将本UVPD方法获得的结果与化合物的式重值进行比较来评估准确度。在 95% 置信水平下基于配对t检验的结果之间没有观察到统计学差异。优化后的 UVPD 方法随后应用于从当地市场购买的一些领先品牌的各种药物和口腔卫生产品（牙膏和漱口水）。