Quantification of antihistamine acrivastine in plasma by solid-phase extraction and high-performance liquid chromatography

Isolation, structure elucidation, and high‐performance liquid chromatography quantification of photolytic degradation impurities in acrivastine

“…The structure of 3 is shown in Figure 2; it is named cis-Δ 7,8 acrivastine. Compound 4 is a reported impurity of acrivastine, and the 1 H and 13 C NMR data (Supporting Information S1 and S2, Tables S1 and S2) agree well with the reported acrivastine Z-isomer [18]. To confirm the configuration of C11═C19, the planar structure of 4 is constructed by detailed analyses of 1 H NMR, 13 C NMR, 1 H 1 H COSY, HSQC, and NOESY (Supporting Information S15-S19).…”

“…Combining the HSQC correlations, the main fragments of 3 were established, and the structure was elucidated (Figure 3). Comparing the 1 H and 13 C NMR data (Supporting Information S1 and S2, Tables S1 and S2) of 3 with those of acrivastine, they are similar, except for H- This can be confirmed by the coupling constant 3 J H7-H8 = 12.8 Hz in 3, but acrivastine with trans C7═C8 configuration has a larger coupling constant of 3 J H7-H8 = 16.0 Hz. The ethylene Δ 11,19 of 3 takes E configuration, which is the same as that of acrivastine.…”

“…The NMR spectra were recorded using Bruker-600 NMR spectrometers operating at 600 and 150 MHz for 1 H and 13 C, respectively, in CDCl 3 or CH 3 OD solvent and tetramethylsilane as internal standard. 2-D NMR experiments were also performed using the same instrument in the same solvent.…”

“…The formula is the same as that of 3, which is also an isomer of acrivastine. The 1 H NMR and 13 C NMR data (Supporting Information S1 and S2, Tables S1 and S2) of 5 are similar to those of 3; the only differences are the up-field shift of H-19 at δ H 6.27 (Δδ 0.63), the down-field shift of C-12 at δ C 137.3 (Δδ 3.7), and C-19 at δ C 128.1 (Δδ 4.4), compared with those of 3. The planar structure of 5 was constructed by detailed analyses of the 1 H 1 H COSY, NOESY, and HSQC spectra (Supporting Information S27-S31), as the same method as 3.…”

Development and validation of an ultra‐performance liquid chromatography method for simultaneous analysis of 20 antihistaminics in dietary supplements

“…A number of methods have been reported in the literature for individual or simultaneous determination of antihistaminic contents in various materials. Multiple high‐performance liquid chromatography (HPLC) methods have been reported (Massart and Detaevernier, ; Kai‐On and Kam‐Chung, ; Martínez‐Algaba et al ., ), including a method for antihistamine quantification in plasma samples (Collins and Gu, ). Additionally, a gas chromatography/mass spectrometry (GC/MS) method that enables simultaneous detection of 10 antihistamines in human plasma has been described (Hasegawa et al ., ).…”