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Abstract

High-performance liquid chromatography with a hydrophilic-interaction liquid chromatographic (HILIC) column has been successfully used to retain and separate the polar phosphonic herbicides glyphosate and glufosinate. Online electrospray tandem ion-trap mass spectrometric and DAD detection were used. The effects on the separation of mobile phase acetonitrile content, buffer concentration, and flow rate, and of column temperature, were investigated. With UV-visible detection at 195 nm, LOQ were <850 mg kg−1, showing the method is suitable for product quality control of these herbicides alone or in combination. Tandem mass spectrometric conditions were optimized for ion-trap detection. Quantification was by use of selected reaction monitoring transitions m/z 168 → 150 in negative-ion mode for glyphosate and m/z 182 → 136 in positive-ion mode for glufosinate. Limits of detection (LOD; S/N > 3) were 0.20 and 0.16 ng for glyphosate and glufosinate, respectively, and the respective limits of quantification (LOQ; S/N = 10) were 0.02 and 0.05 mg kg−1. Sample derivatization was not necessary to achieve low detection limits in residue analysis in this study. Recovery from watermelon, spinach, potato, tomato, radish-root, and water fortified with the herbicides ranged from 63.6 to 107.3% and relative standard deviations were <15.3%.

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Cortisol and cortisone are 2 important glucocorticoids produced in the human hypothalamus–pituitary–adrenal (HPA) axis that respond to stress. An analytical method to determinate cortisol and cortisone in serum and saliva using high-performance liquid chromatography–tandem mass spectrometry following a supported liquid extraction (SLE) was developed. Serum and saliva samples of 0.2 mL were extracted by SLE three times using 0.4 mL of methyl tert-butyl ether each time. The chromatographic separation was obtained on an Agilent Poroshell column using a 0.01% formic acid buffer and acetonitrile (60:40, v/v) as the solvent with a flow rate of 0.3 mL/min. Optimized quantitative mass transitions for cortisol, cortisone, and cortisone d-4 were 363.2/121.0 (m/z), 361.2/163.1 (m/z), and 367.1/270.7 (m/z), respectively. The method validation was achieved according to regulatory guidance. The lower limit of quantification (LLOQ) in serum were 2 ng/mL for cortisol and 1 ng/mL for cortisone, and the LLOQ in saliva were 0.1 ng/mL for cortisol and 0.2 ng/mL for cortisone. The developed method showed convenient and efficient extraction, a lower LLOQ, and a short running time. Modest correlations between serum and saliva cortisol and cortisone concentrations were found. The method was successfully applied in assessing the HPA condition of patients with depressive disorders.

Open access

Abstract

A rapid and sensitive High-Performance Liquid Chromatography-tandem Mass Spectrometry (HPLC/MS/MS) method for determining apremilast in beagle dog plasma and urine samples was developed and validated using clopidogrel as the internal standard (IS). Apremilast was extracted from the plasma and urine samples by liquid–liquid extraction using methyl tert-butyl ether. Chromatographic separation was performed using a C8 column with gradient elution and a mobile phase containing methanol and 0.1% formic acid. Quantification was achieved in multiple reaction monitoring (MRM) mode with a transition of m/z 461.3→178.2 for apremilast and m/z 322.2→184.1 for clopidogrel (IS). This method was validated regarding its specificity, linearity, precision, accuracy, and stability. The lower limit of quantification (LLOQ) for this method was 5 ng/mL, and the calibration curve was linear over 5–1,000 ng/mL. The intra- and inter-run coefficients of variance (CV) of aprelimast in plasma samples were less than 12.92% and 10.64%, respectively, while in urine samples, the CV were less than 11.84% and 10.20%, respectively. The samples were stable under the tested conditions. This method was successfully applied to a pharmacokinetic study in beagle dogs following oral administration of 10 mg of apremilast.

Open access
Acta Chromatographica
Authors: Weijian Ye, Wei Sun, Ruijie Chen, Zhe Wang, Xiao Cui, Hui Zhang, Shuyi Qian, Qi Zheng, Yangfeng Zhou, Jiafeng Wan, Jiali Xu, Xianqin Wang, and Yunfang Zhou

Galangin (GAL), the major bioactive flavonol extracted from Alpinia officinarum Hance (Zingiberaceae), has attracted much attention due to its multiple biological activities. To develop a fast, reliable, and sensitive ultrahigh-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method for the quantification of GAL in rat plasma and mouse tissues. UHPLC–MS/MS using electrospray ionization operating in negative-ion mode was used to determinate GAL in 18 rats receiving three doses of GAL (2 and 9 mg/kg by intravenous injection, 5 mg/kg by oral administration), with six rats for each dose. Blood samples were collected at 0.0333, 0.25, 0.5, 1, 2, 4, 6 and 8 h. A total of 25 mice received 18 mg/kg GAL by intraperitoneal injection. Liver, heart, lung, spleen, brain, and kidney tissue samples were collected at 0.25, 0.5, 2, 4, and 6 h. The precision of the method was better than 12.1%, while the accuracy ranged from −4.8% to 8.1%. The results of pharmacokinetics demonstrated rapid GAL absorption (t max of 0.25 h), fast elimination (t 1/2 <1.1 h) after three different dosages, and an absolute bioavailability of ~7.6%. Tissue distribution analysis revealed abundant GAL in liver, kidney, spleen, and lung and smaller amounts in brain. The developed method proved fast (3 min), efficient, and reliable, with high selectivity for the quantitative analysis of GAL in biological samples. This is the first study to identify the target tissues of GAL, and the results may help to elucidate the mechanisms underlying its therapeutic effects in vivo.

Open access

Abstract

Background and aims

Due to the rapid spread of the novel coronavirus disease 2019 (COVID-19), policies based on the nature of “spatial distancing” have been implemented and have resulted in school suspensions and online learning among schoolchildren. In order to examine the impact of such policies on schoolchildren, the aims of the present study were to (i) assess changes in the level of engagement in three internet-related activities (smartphone use, social media use, and gaming) before and during the COVID-19 outbreak, including prolonged and problematic engagement in these activities; (ii) investigate the differences of psychological distress before and after COVID-19 outbreak; and (iii) to use structural equation modeling to investigate the mediating roles of problematic internet-related behaviors in the causal relationships of psychological distress and time spent on internet-related activities.

Methods

Self-report measures were used to assess internet-related activities and psychological distress. Time spent on internet-related activities, problematic use of internet-related activities, and psychological distress were collected from primary school students (N = 535; 265 boys; M age = 10.32 years [SD = 0.84]). The data were first collected before the COVID-19 outbreak (i.e., early November 2019) and then collected again during the school suspension due to COVID-19 outbreak (i.e., end of March 2020) for comparisons of changes.

Results

Schoolchildren spent significantly more time on the smartphone (increased 1.02 h daily; P < 0.001) and social media (increased 0.73 h daily; P < 0.001) but not gaming (increased 0.14 h daily; P = 0.07) during the school suspension compared to the baseline. Schoolchildren who increased by 15 or 30 min daily on internet-related activities showed an increased level of psychological distress. The association between problematic use of social media and psychological distress was stronger during the school suspension (β = 0.584) than at the baseline (β = 0.451; P < 0.001).

Conclusion

Increased problematic use of internet-related activities among schoolchildren was associated with greater psychological distress. Parents should therefore monitor internet-related activities and psychological distress of their children to support their mental health.

Open access
Journal of Behavioral Addictions
Authors: Tao Luo, Lixia Qin, Limei Cheng, Sheng Wang, Zijun Zhu, Jiabing Xu, Haibo Chen, Qiaosheng Liu, Maorong Hu, Jianqin Tong, Wei Hao, Bo Wei, and Yanhui Liao

Abstract

Objective

Social media disorder (SMD) is an increasing problem, especially in adolescents. The lack of a consensual classification for SMD hinders the further development of the research field. The six components of Griffiths’ biopsychosocial model of addiction have been the most widely used criteria to assess and diagnosis SMD. The Bergen social media addiction scale (BSMAS) based on Griffiths’ six criteria is a widely used instrument to assess the symptoms and prevalence of SMD in populations. This study aims to: (1) determine the optimal cut-off point for the BSMAS to identify SMD among Chinese adolescents, and (2) evaluate the contribution of specific criteria to the diagnosis of SMD.

Method

Structured diagnostic interviews in a clinical sample (n = 252) were performed to determine the optimal clinical cut-off point for the BSMAS. The BSMAS was further used to investigate SMD in a community sample of 21,375 adolescents.

Results

The BSMAS score of 24 was determined as the best cut-off score based on the gold standards of clinical diagnosis. The estimated 12-month prevalence of SMD among Chinese adolescents was 3.5%. According to conditional inference trees analysis, the criteria “mood modification”, “conflict”, “withdrawal”, and “relapse” showed the higher predictive power for SMD diagnosis.

Conclusions

Results suggest that a BSMAS score of 24 is the optimal clinical cut-off score for future research that measure SMD and its impact on health among adolescents. Furthermore, criteria of “mood modification”, “conflict”, “withdrawal”, and “relapse” are the most relevant to the diagnosis of SMA in Chinese adolescents.

Open access