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A sensitive, stability-indicating reversed-phase high-performance liquid chromatography with diode array detection (HPLC–DAD) method has been developed for the determination of TBI-166 and its 10 kinds of related impurities. Chromatographic separation was achieved on a Kromasil ODS column (250 mm × 4.6 mm, 5 μm), with a gradient elution of the mobile phase system consisting of acetonitrile and 1% ammonium formate solution (with 0.2% formic acid). The flow rate was 1.0 mL/min, and the detection wavelength was set at 251 nm. The method was validated according to the International Conference on Harmonization (ICH) guidelines with respect to selectivity, linearity, limits, accuracy, precision, and robustness. The calibration curves were linear from LOQ to 150% of the specification limit of impurity with correlation coefficients not less than 0.999. The limits of quantitation were between 0.123 and 0.257 μg/mL. Accuracy for the related substances was estimated by the recovery ranged from 94.6% to 111.2%. The method was proved to be reliable for the determination of related substances in TBI-166 bulk drug, which is essential and important in the quality control.

Open access
Acta Chromatographica
Authors: Yun Wang, Jianhong Chen, Yutian Li, Puling Li, Javed Iqbal, Ying Chen, Yinlian Ma, and Cun Zhang

A reliable and rapid high-performance liquid chromatography coupled with diode array detector method (HPLC–DAD) was established and validated to determine eight gingerol simultaneously in the rhizomes of Zingiber offcinale Rosc. The separation of eight compounds (4-hydroxy-3-methoxy-benzenebutanol,3,5-dihydroxy-1-(4-hydroxy-3-methoxyphenyl) decane, 3,5-dihydroxy-1-(3,4-dimethoxyphenyl) decane, 6-gingerol, 8-gingerol, 6-shogaol, 5-hydroxy-1-(4-hydroxy-3-methoxyphenyl)-1,4-decadien-3-one, and 10-gingerol) were performed on an Agilent TC(2) C18 (250 mm × 4.6 mm, 5 μm) at 30 °C using acetonitrile (A) and 1% formic acid aqueous solution (B) as the mobile phase with gradient elution (0–10 min, 20%–35% A; 10–28 min, 35%–55% A; 28–35 min, 55%–60% A; 35–55 min, 60%–70% A; 55.01–60 min, 100%–100% A). The detection wavelength was set at 280 nm, and the flow rate was 0.8 mL/min. Validation of the analytical method was performed by linearity, precision, and accuracy test. All compounds were quantified with good linear calibration curves (coefficient of determination R 2, >0.9999). The method showed good precision with overall coefficients of variation between 0.56% and 0.84%. The range of recovery was from 95.50% to 104.14% for the analytes. This method was successfully applied to quantify eight gingerols in Z. offcinale Rosc from different regions in China, so it can provide quality assessment for this medicine.

Open access

RKI-1447 is an effective ROCK1 and ROCK2 inhibitor, having anti-invasion and anti-tumor activity. In this study, we used ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) to detect RKI-1447 in rat plasma and investigated its pharmacokinetics in rats. Diazepam was utilized as an internal standard, and an acetonitrile precipitation method was used to process the plasma samples. Chromatographic separation was achieved using a UPLC ethylene bridged hybrid (BEH) column (2.1 mm × 50 mm, 1.7 μm) with a gradient acetonitrile–water mobile phase (containing 0.1% formic acid). Flow rate was set at 0.4 mL/min. Electrospray ionization (ESI)–tandem mass spectrometry in multiple reaction monitoring (MRM) mode with positive ionization was applied: m/z 327.1 → 204.0 and 285.1 → 193.3 for RKI-1447 and internal standard, respectively. The results indicated that within the range of 10–2000 ng/mL, the linearity of RKI-1447 in rat plasma was acceptable (r > 0.995), and the lowest limit of quantification (LLOQ) was 10 ng/mL. Intra-day precision RSD of RKI-1447 in rat plasma was lower than 8%, and inter-day precision RSD was lower than 11%. Accuracy range was between 91.6% and 107.1%, and the matrix effect was between 85.1% and 87.0%. The analysis method was sensitive and fast with suitable selectivity, and was successfully applied in the pharmacokinetics of RKI-1447 in rats. The bioavailability of the RKI-1447 was 7.3%.

Open access

A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method and ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC–MS/MS) were optimized and validated for 16 antibiotics belonging to three families (macrolides, quinolones, and sulfonamides) that were found in preserved eggs. Samples were extracted in 4 mL water and 10 mL acetonitrile with 1% acetic acid and subjected to a cleanup procedure using dispersive solid-phase extraction with C18 and primary secondary amine sorbents, prior to detection by UHPLC–MS/MS. Matrix-matched calibration was used for quantification to reduce the matrix effect with limits of quantification in the range of 0.3–3.0 μg/kg. Validation of the method was conducted by recovery and precision experiments. Recoveries of the spiked samples ranged from 73.8% to 127.4%, and the intra- and inter-day relative standard deviations were lower than 21.2% and 22.3%, respectively. This method was successfully applied to the analysis of antibiotics in preserved egg samples.

Open access

Abstract

The aim of the experiment is to establish a method for the determination of acrylamide in food by automatic accelerated solvent extraction-gas chromatography-mass spectrometry. D3-acrylamide was used as isotope internal standard, crushed samples were extracted and purified by automatic accelerated solvent, acrylamide was derivatized into 2,3-dibromopropanamide by potassium bromide and potassium bromate under acidic conditions, and then the derivative was extracted by ethyl acetate and detected by gas chromatography-mass spectrometry. The method had a good linear relationship in the concentration range of 10–2000 ng/mL, and the coefficient of determination (R2) was 0.9997. The detection limit of the method was 3 μg/kg. The quantification limit of the method was 10 μg/kg. The standard addition recovery of acrylamide was between 105 and 120%, and the relative standard deviation of the recovery of acrylamide was less than 3.0%. The experimental result showed that the method was simple, sensitive, efficient and accurate, and could be used for the determination of acrylamide in food.

Open access

Summary

A reversed-phase chiral liquid chromatographic method had been developed and validated for resolution of the enantiomers of racemic fudosteine. The effects on the separation of the amounts of anhydrous cupric sulfate and l-phenylalanine, the methanol content, mobile phase pH, and temperature were investigated. The method was validated for linearity, repeatability, intermediate precision, sample recovery, solution stability, and limits of detection (LOD). l-Phenylalanine and anhydrous cupric sulfate as chiral ligand-exchange complexes were used for separation, isomer identification, related substance investigation, and analysis of fudosteine enantiomers in fudosteine bulk drugs and fudosteine tablets.

Full access
Journal of Behavioral Addictions
Authors: Haoran Meng, Hongjian Cao, Ruining Hao, Nan Zhou, Yue Liang, Lulu Wu, Lianjiang Jiang, Rongzi Ma, Beilei Li, Linyuan Deng, Zhong Lin, Xiuyun Lin, and Jintao Zhang

Abstract

Background and aims

Previous studies on smartphone use motivation (SUM) and problematic smartphone use (PSU) have been limited in the utilization of regional samples of emerging adults (e.g., college students) and also in the foci on the direct association between SUM and PSU. To address such gaps, using data from a large, national representative sample of Chinese young adolescents and their parents this study examined the associations between adolescents' various types of SUM and their PSU, and also tested the potential mediating roles of smartphone use time (SUT) that adolescents spent on various activities in such associations.

Methods

A nationwide representative sample of 8,261 Chinese adolescents (Mage = 12.86 years old, SD = 1.76; 42.6% females) and their parents (49% mothers) participated in this survey study.

Results

Instrumental SUM (i.e., to expand knowledge or acquire information) was associated negatively with PSU via longer SUT spent on learning and shorter SUT spent on entertainment and communication. Self-expression SUM (i.e., to gain acceptance and recognition of others by maintaining or improving self-images) was associated with longer SUT spent on both learning and entertainment, which, in turn, predicted lower and higher levels of PSU, respectively. Last, hedonic SUM (i.e., to gain pleasure) was associated positively with PSU via longer SUT spent on entertainment and communication.

Discussion

These findings contribute to the literature by adding greater specificity in our understanding of the implications of SUM and SUT in the etiology of PSU during the critical life stage of adolescence in a Chinese cultural context.

Open access
Journal of Behavioral Addictions
Authors: Shan-Shan Ma, Chiang-Shan R. Li, Sheng Zhang, Patrick D. Worhunsky, Nan Zhou, Jin-Tao Zhang, Lu Liu, Yuan-Wei Yao, and Xiao-Yi Fang

Abstract

Background and aims

Deficits in cognitive control represent a core feature of addiction. Internet Gaming Disorder (IGD) offers an ideal model to study the mechanisms underlying cognitive control deficits in addiction, eliminating the confounding effects of substance use. Studies have reported behavioral and neural deficits in reactive control in IGD, but it remains unclear whether individuals with IGD are compromised in proactive control or behavioral adjustment by learning from the changing contexts.

Methods

Here, fMRI data of 21 male young adults with IGD and 21 matched healthy controls (HC) were collected during a stop-signal task. We employed group independent component analysis to investigate group differences in temporally coherent, large-scale functional network activities during post-error slowing, the typical type of behavioral adjustments. We also employed a Bayesian belief model to quantify the trial-by-trial learning of the likelihood of stop signal – P(Stop) – a broader process underlying behavioral adjustment, and identified the alterations in functional network responses to P(Stop).

Results

The results showed diminished engagement of the fronto-parietal network during post-error slowing, and weaker activity in the ventral attention and anterior default mode network in response to P(Stop) in IGD relative to HC.

Discussion and conclusions

These results add to the literatures by suggesting deficits in updating and anticipating conflicts as well as in behavioral adjustment according to contextual information in individuals with IGD.

Open access