[Pharmaceutical Ingredients Detected in Dietary Supplements Purchased by Chiba Prefecture (Fiscal Years 2014-2021)].

In the pharmaceutical ingredients contamination testing of 702 commercial dietary supplement products, during fiscal years 2014-2021, 14 pharmaceutical ingredients, barrenwort, leaf axils of senna, and small leaf of senna were detected in 28 products. Screening and confirmation of the pharmaceutical ingredients in the products were performed by ultra-high performance liquid chromatography with photodiode array detector and ultra-high performance liquid chromatography-quadrupole-kingdon trap mass spectrometry, respectively. In particular, leaf axils and small leaf of senna were identified by stereomicroscopy and scanning electron microscopy. Furthermore, we found several pharmaceutical ingredients that exceeded the daily medicated dosage; therefore, it is important to prevent the distribution of such products to prevent the occurrence of health hazard. For that reason, it is necessary to continue the sample purchasing and testing systems to monitor the distribution of products containing pharmaceutical ingredients.

[The Configuration of Tadalafil and Tadalafil Analogues Found in Dietary Supplements].

This study determined the configuration of the isomers of tadalafil, nortadalafil, and homotadalafil in dietary supplements. The products purchased over the Internet studied included a honey product and a tablet, which contained tadalafil, and a candy, which contained nortadalafil and homotadalafil. Each of the pharmaceutical ingredients isolated from the products was measured with circular dichroism (CD).As a result, the CD spectrum of each isolated pharmaceutical ingredient was found to align with the standard CD spectrum of the 6R,12aR isomer, confirmed that each isolated tadalafil or tadalafil analogue included in a 6R,12aR isomer. According to a report, among the stereoisomers of tadalafil, the 6R,12aR isomers have the most potent inhibitory activities of phosphodiesterase-type-5. From the report, the potential strength of the inhibitory activity of the 6R,12aR isomers of nortadalafil and homotadalafil was suggested. Therefore, it seemed that the 6R,12aR isomer often used in the product.

Air segmented amplitude modulated multiplexed flow analysis with software-based phase recognition: determination of phosphate ion.

Amplitude modulated multiplexed flow analysis (AMMFA) has been improved by introducing air segmentation and software-based phase recognition. Sample solutions, the flow rates of which are respectively varied at different frequencies, are merged. Air is introduced to the merged liquid stream in order to limit the dispersion of analytes within each liquid segment separated by air bubbles. The stream is led to a detector with no physical deaeration. Air signals are distinguished from liquid signals through the analysis of detector output signals, and are suppressed down to the level of liquid signals. Resulting signals are smoothed based on moving average computation. Thus processed signals are analyzed by fast Fourier transform. The analytes in the samples are respectively determined from the amplitudes of the corresponding wave components obtained. The developed system has been applied to the simultaneous determinations of phosphate ions in water samples by a Malachite Green method. The linearity of the analytical curve (0.0-31.0 µmol dm(-3)) is good (r(2)>0.999) and the detection limit (3.3 σ) at the modulation period of 30s is 0.52 µmol dm(-3). Good recoveries around 100% have been obtained for phosphate ions spiked into real water samples.