Transfer of seven thin-layer chromatography (TLC) Global Pharma Health Fund E.V. Minilab protocols for screening counterfeit pharmaceutical products in the field to quantitative high-performance TLC (HPTLC)–densitometry methods was performed using a model process published previously. The developed and validated methods for tablets containing amlodipine besylate, cefpodoxime proxetil, cetirizine 2HCl, diclofenac sodium, efavirenz, mefenamic acid, and atovaquone + proguanil HCl involved the use of only relatively inexpensive and nontoxic solvents, Merck KGaA Premium Purity HPTLC silica gel 60 F254 plates, semi-automated sample and standard solution application with a CAMAG Linomat 4, and automated densitometry with a CAMAG Scanner 3 for detection, identification, and quantification. In addition, previously transferred HPTLC–densitometry methods for azithromycin and for cephalexin were used to analyze a new product of each drug to demonstrate the applicability of the methods.
High-performance thin-layer chromatography (HPLTC)–densitometry methods are described for the analysis of the anti(retro)virals dolutegravir (D), lamivudine (L), and tenofovir disoproxil fumarate (TDF) in a pharmaceutical tablet product. To the best of our knowledge, no previous quantitative planar chromatography method has been reported in the literature for this combination formulation. The method for L was transferred from a thin-layer chromatography (TLC) screening method published in the Global Pharma Health Fund (GPHF) Minilab Manual designed for identification of counterfeit and substandard drug products using a model process published earlier. D and TDF are not included in the list of drugs for which TLC screening methods are published for the Minilab, but HPTLC–densitometry procedures were developed for them using the transfer process guidelines. L was analyzed simultaneously with TDF on Merck Premium Purity silica gel 60 F plates using the mobile phase ethyl acetate–methanol–acetone–concentrated ammonium hydroxide (30:7:3:1) and densitometric scanning at 254 nm. D was analyzed on a second plate by scanning at 366 nm after chromatography with the chloroform–methanol–formic acid (32:8:2) mobile phase. Data for all three drugs are shown to meet the requirements of the model transfer process for calibration curve r values, assay of tablets relative to their label values, peak purity/peak identity tests, and validation by standard addition analysis of samples spiked at 50%, 100%, and 150% of the label value of active ingredients. A TLC screening method for TDF in the combination product was developed and published online with open access.
227Ac,228Th,226Ra,210Po and210Pb can be present at rare earth chlorides. A radiochemical procedure is presented for the identification and determination of natural radioactive impurities in rare earth chlorides. The determination limits for these radionuclides were 1.5·10–4 to 3·10–1 Bq/g. The relative standard deviations for determining 10–2 Bq/g radionuclides were usually less than ±7%.
Authors:Y. Lou, Y. Rhee, H. Yen, Y. Gu, H. Cao, J. Yuan, and Y. Jean
The two-dimensional angular correlation of annihilation radiation (2D-ACAR) technique has been developed to measure the hole structure of stretched and oriented polymers. The determination of polymer hole structure is demonstrated in a stretched semi-crystalline polyaryl-ether-ether-ketone (PEEK) sample. The atomic scale anisotropy is found to be consistent with the macroscopic scale stretch ratio. Applications of the 2D-ACAR method to image the three-dimensional hole, free-volume, and cavity structures of molecular systems are discussed.
Authors:J. Du, H. Song, D. Mu, D. Li, S. Yan, and Y. Gu
The sorption/desorption of radioruthenium was investigated by the batch method in sea water system at ambient temperature
on the surface sediments obtained around the Daya Bay of Guangdong Province, where the first nuclear power station of China
has been running from 1994. It was found that the sorption percentage was obtained to be around 40% for all the surface sediments
in 60 minutes. Then, the sorption percentage goes up slowly. The sorption percentage of radioruthenium reached around 80%
in 113 days (2713 hours). The distribution coefficients decreased from 3.16·104 to 1.35·103 ml/g with the increasing of sediment concentration in the range of 4–10000 mg/l. The results of the desorption experiments
suggest that the sorption of radioruthenium is irreversible with 81.5% relative hysteresis coefficient.
Authors:D. Mu, H. Song, S. Yan, Y. Gu, D. Li, and J. Du
Three kinds of marine bivalves (wild Saccostrea cucullata, aquacultured Perna viridis and aquacultured Pinctada martens), collected from Daya Bay, the South China Sea, were used to investigate the bio-accumulation of radioruthenium in the glass
aquarium with natural seawater (pH 8.20, 35‰ salinity, filtered by 0.45 μm) at ambient temperature under laboratory feeding
conditions. The experimental results show that the stead-state of biology concentration factor (BCF, ml/g) of radioruthenium
was approached around 6 days for most species of bivalves. The values of BCF in shells are the highest in organs all the three
bivalves. The orders of BCF values (ml·g−1) are as: Perna viridis (33.2) < Saccostrea cucullata (47.0) < Pinctada martensi (208.4) for shells and Saccostrea cucullata (1.5) < Pinctada martensi (2.2) ≈ Perma viridis (2.4) for soft tissues, respectively, after exposed for 14 days. The rate constants of uptake and elimination of radioruthenium
on marine bivalves were also discussed by first-order kinetics model. The Pinctada martensi may be applicable to be an indicator for monitoring radioruthenium among the three bivalves.
Authors:A. He, M. Ye, Z. Tang, S. Lu, Y. Gu, X. Fan, L. Zhao, and J. Gao
The recombination of hydrogen and oxygen in technical gaseous waste of nuclear power plants in enlarged scale experiment has
been studied on the basis of our previous work.1 The catalyst and its best operating conditions for recombination of hydrogen and oxygen determined in a small scale experiment
were demonstrated and tested. The results show that the data obtained in an enlarged scale experiment agreed well with that
of in a small scale test. The recombination rate of H2 and O2 was higher than 98.3% and 99.98% respectively. After recombination, the residual concentrations of H2 and O2 in waste gas were O2<3 ppm, H2<400 ppm. The Pd-Al2O3 catalyst and operating conditions determined for gaseous waste processing of nuclear power plants were satisfactory.
Authors:D. H. Mu, J. Z. Du, D. J. Li, H. Q. Song, S. P. Yan, and Y. J. Gu
The comprehension of the behavior of radioactive nuclides in aquifer requires the study of the sorption processes of nuclides
in various geochemical conditions. The sorption/desorption of 65Zn(II) on surface sediments (0-2 cm) was investigated by batch method in sea water (pH 8.20, 35‰ salinity, filtered by 0.45mm)
at ambient temperature. The surface sediments were obtained from four stations around the Daya Bay of Guangdong Province (China),
where the first nuclear power station of China has been running from 1994. The sorption process is fast initially and around
39% average of sorption percentage (SP%) can be quickly obtained in 15 minutes for all the surface sediments. Then, the sorption
percentage becomes constant. In 30 days of contact time 79.6% sorption percentage and Kd=3.9. 103ml/g distribution coefficient was obtained. The value of Kdbecame constant, 4.0. 103ml/g, in contact time more than 120 hours. The distribution coefficient Kddecreases with increasing sediment concentration from 4.0 to 250 mg/l from 1.31. 104to 1.68. 103ml/g, respectively. Then the value of Kdgoes up to 5.38. 103ml/g with sediment concentration of 3000 mg/l. The desorption experiments suggest that the sorption of Zn(II) is irreversible
with a hyteresis coefficient of 66%.
Authors:Y.P. Jing, D.T. Liu, X.R. Yu, F. Xiong, D.L. Li, Y.K. Zheng, Y.F. Hao, Y.J. Gu, and Z. Wang
The objective of the present study was to understand the developmental regularity of wheat endosperm cells at different Days After Pollination (DAP) using microscopic and histochemical methods. Resin semi-thin sections of the endosperm and the enzymatically dissociated Starchy Endosperm Cells (SECs) were observed under a light microscope. The results showed that: (1) SECs were irregular-shaped and had two types of starch granules: large oval-shaped A-type starch granules and small spherical B-type starch granules. (2) The growth shape of SECs was referred to as S-curve and the fastest cell growth period was at 16–24 DAP. (3) The largest increase and growth of A-type starch granules were mainly at 4–16 DAP. B-type starch granules increased rapidly after 16 DAP and made up over 90% of the total starch granules in SEC during the late stage of endosperm development. (4) The nuclei of SEC deformed and degenerated during the middle and late stages of endosperm development and eventually disappeared. However, starch granules still increased and grew after the cell nuclei had degenerated. The investigations showed the development regularity of starch endosperm cells and starch granules, thereby improving the understanding of wheat endosperm development.
Authors:W.-C. Xie, X.-H. Gu, Z.-C. Tan, J. Tang, G.-Y. Wang, C.-R. Luo, and L.-X. Sun
To develop thermal stable flavor, two glycosidic bound flavor precursors, geranyl-tetraacetyl-β-D-glucopyranoside (GLY-A) and geranyl-β-D-glucopyranoside (GLY-B) were synthesized by the modified Koenigs–Knorr reaction. The thermal decomposition process and pyrolysis products of the two glycosides were extensively investigated by thermogravimetry (TG), differential scanning calorimeter (DSC) and on-line pyrolysis-gas chromatography mass spectroscopy (Py-GC-MS). TG showed the Tp of GLY-A and GLY-B were 254.6 and 275.7°C. The Tpeak of GLY-A and GLY-B measured by DSC were 254.8 and 262.1°C respectively.
Py-GC-MS was used for the simply qualitative analysis of the pyrolysis products at 300 and 400°C. The results indicated that: 1) A large amount of geraniol and few by-products were produced at 300°C, the by-products were significantly increased at 400°C; 2) The characteristic pyrolysis product was geraniol; 3) The primary decomposition reaction was the cleavage of O-glycosidic bound of the two glycosides flavor precursors. The study on the thermal behavior and pyrolysis products of the two glycosides showed that this kind of flavor precursors could be used for providing the foodstuff with specific flavor during heating process.