Dziurkowska Ewelina, Wesolowski Marek
Department of Analytical Chemistry, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk, Poland.
J Clin Med. 2020 Mar 27;9(4):915. doi: 10.3390/jcm9040915.
Saliva is a valuable diagnostic material that, in some cases, may replace blood. However, because of its different composition, its use requires the development of new, or the modification of existing, extraction procedures. Therefore, the aim of the study was to develop a method of saliva purification that would enable the determination of carbamazepine and its metabolite, carbamazepine-10,11 epoxide. When comparing two methods of sample purification (Solid Phase Extration (SPE) and deproteinization), it was found that the second method yielded more favorable results. A 1% formic acid solution in acetonitrile was used for extraction. The samples were shaken and centrifuged, and the supernatant obtained was evaporated and dissolved in a mobile phase, then chromatographically analyzed. The developed method was validated by determining its linearity in the range of 10-5000 ng/mL for both analytes. Intra- and inter-day precision did not exceed 14%. In order to check the usefulness of the method, both analytes were determined in the saliva samples from 20 patients treated with carbamazepine. The content of both analytes was detected and determined in all of the tested samples of saliva. It was found that the method developed is rapid, sensitive, reliable, and can be used to monitor the concentration of carbamazepine and metabolite in patients' saliva.
唾液是一种有价值的诊断材料，在某些情况下可替代血液。然而，由于其成分不同，使用时需要开发新的提取程序或对现有程序进行改进。因此，本研究的目的是开发一种唾液纯化方法，以便能够测定卡马西平及其代谢物卡马西平-10,11-环氧化物。在比较两种样品纯化方法（固相萃取（SPE）和去蛋白）时，发现第二种方法产生了更有利的结果。使用乙腈中的1%甲酸溶液进行萃取。将样品振荡并离心，所得上清液蒸发并溶解于流动相中，然后进行色谱分析。通过测定两种分析物在10-5000 ng/mL范围内的线性来验证所开发的方法。日内和日间精密度均不超过14%。为了检验该方法的实用性，对20名接受卡马西平治疗的患者的唾液样本中的两种分析物进行了测定。在所有测试的唾液样本中均检测并测定了两种分析物的含量。结果发现，所开发的方法快速、灵敏、可靠，可用于监测患者唾液中卡马西平及其代谢物的浓度。
