Development of a LC.MS/MS method for simultaneous analysis of 20 antihistamines in dietary supplements

Abstract

Recently, the consumption of dietary supplements has increased because of people's greater interest in health. Unfortunately, the sales of dietary supplements containing unauthorized substances such as drugs have also increased. We developed a rapid, accurate method for the simultaneous determination of antihistamines using liquid chromatography tandem mass spectrometry with a multiple reaction monitoring mode. The limit of detection (LOD) and limit of quantification (LOQ) of the instrument used in this method were in the ranges 0.0003-0.3 and 0.0009-0.6 µg mL −1 , respectively. The linearity of the method was > 0.99. The precision levels of the method were 0.1-9.8% (intra-day) and 0.3-9.6% (inter-day), and the levels of accuracy of the method were 82.7-115.0% (intra-day) and 84.3-113.0% (inter-day). The mean of recovery of the method was in the range of 83.9-117.9% and the RSD of the stability was less than 5.9%.

Pharmacokinetic Comparison of Epinastine Using Developed Human Plasma Assays

“…The most abundant fragment ion for multiple reaction monitoring (MRM) was m/z 249.8 → 193.1 for epinastine and m/z 367.9 → 294.2 for the IS, respectively. The mass spectra results of epinastine were the same as those of Do et al [9] and Bae et al [10]. Figure 1 presents the relevant mass spectra.…”

“…Several studies have used HPLC method for analysis of bulk drug [11], formulation [17], or dietary supplements [9], but are rarely used for biological sample analysis. In addition, the LLOQ values they presented were so high that it was very limited for application in quantifying biological samples.…”

“…The HPLC-UV analysis of epinastine reported by Malakar et al [17] was also for the pharmaceutical dosage form, and the LLOQ was very high as 2 µg/mL. Do et al [9] reported the simultaneous analysis of 20 antihistamines, including epinastine, in dietary supplements, but it was very limited to be directly applied for the analysis of biological samples in consideration of different sample preparation and assay validation and long analysis time per sample. In addition, LLOQ was as high as 90 ng/mL and was not suitable for the analysis of biological samples.…”