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Abstract

The study was aimed to validate and optimize high performance liquid chromatographic (HPLC) method for the determination of coumarin-3-carboxylic acid (C3A) in the heart and liver issue of Sprague-Dawley (SD) rats after intragastric administration of extractive of leaves of Ficus virens var sublanceolata. And simple ADME and target prediction analyses were performed for C3A. Ethyl acetate was employed to precipitate protein with appropriate sensitivity and acceptable matrix effects. The satisfactory separation was developed on an ODS2 column (4.6 mm × 250 mm, 5 μm) by gradient elution with a methanol-acetic acid solution (pH = 3.0) as the mobile phase. The flow rate was 1.0 mL min−1, the column temperature was maintained at 30 ± 2 °C, the injection volume was 20 μL, and the detection wavelength was set as 309 nm. The method was fully validated in terms of selectivity, linearity, accuracy, precision, extraction recovery and stability. The results of the ADME analysis found that C3A has excellent characteristics of drug-likeness, consistent with good bio-absorption. And the predicted 12 target protein belongs to the amine oxidoreductase and carbonic anhydrase target class. This method is simple, rapid, sensitive, and accurate for the determination of coumarin-3-carboxylic acid in the heart and liver tissue of SD rats.

Open access
Acta Chromatographica
Authors:
Peiwu Geng
,
Jing Zhang
,
Bingbao Chen
,
Qianqian Wang
,
Shuanghu Wang
, and
Congcong Wen

Dauricine is the major bioactive component isolated from the roots of Menispermum dauricum D.C., a bisbenzylisoquinoline alkaloid derivative, and has shown multiple pharmacological properties. In this work, a sensitive and selective ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed for determination of dauricine in rat plasma and its application to pharmacokinetic study of dauricine after intravenous and oral administration in rats. After addition of daurisoline as an internal standard (IS), protein precipitation by acetonitrile was used to prepare samples. Chromatographic separation was achieved on a UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) with 0.1% formic acid and acetonitrile as the mobile phase with gradient elution. An electrospray ionization source was applied and operated in positive ion mode; multiple reactions monitoring (MRM) mode was used for quantification. Calibration plots were linear throughout the range 2–600 ng mL−1 for dauricine in rat plasma. Relative standard deviation (RSD) of intra-day and inter-day precision was less than 13%. The accuracy of the method was between 95.8% and 105.9%. Matrix effect of dauricine in rat plasma ranged from 88.0% to 90.3%. Mean recoveries of dauricine in rat plasma ranged from 91.5% to 95.1%. The method was successfully applied to pharmacokinetic study of dauricine after intravenous and oral administration in rats. The bioavailability of dauricine was found to be 55.4% for the first time.

Open access
Acta Chromatographica
Authors:
Shuanghu Wang
,
Zixia Lin
,
Ke Su
,
Jing Zhang
,
Lijing Zhang
,
Zhimou Gao
,
Zhiyi Wang
,
Jianshe Ma
, and
Xianqin Wang

The rats were randomly divided into paraquat group, curcumin treatment group, and pirfenidone treatment group. The concentration of paraquat in rat plasma was determined by an ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method over the range of 10–2000 ng mL−1. Chromatographic separation was achieved on a BEH HILIC (2.1 mm × 100 mm, 1.7 μm) column. The mobile phase was consisted of acetonitrile and 10 mm ammonium formate buffer (containing 0.1% formic acid) with gradient elution pumped at a flow rate of 0.4 mL min−1. Protein precipitation with acetonitrile was used as sample preparation. Compared with the paraquat group, there is statistical toxicokinetic difference for curcumin treatment group and pirfenidone treatment group, AUC(0 − t) decreased (P < 0.05), clearance (CL) increased (P < 0.05) for curcumin or pirfenidone treatment group, and C max decreased (P < 0.05) for curcumin treatment group. The results showed that treatment by curcumin and pirfenidone could relieve acute paraquat poisoning in rats.

Open access

Abstract

Letrozole is one of the third generation aromatase inhibitors. It is suitable for the treatment of postmenopausal patients with advanced breast cancer and early treatment of breast cancer. It is necessary to develop a rapid, reliable, selective and sensitive LC–MS/MS assay to determine letrozole in human plasma to evaluate the clinical efficacy and adverse reactions with clinical pharmacokinetic and therapeutic drug monitoring. Separation was carried out on a Kromasil-C18 column using acetonitrile-water (55: 45, v/v) as mobile phase. Detection was carried out by multiple reaction monitoring on a 3200Qtrap mass spectrometry. The method needed one-step protein precipitation procedure only, and the cycle time was 2.5 min allowing 500–550 samples per day. It was linear within 0.30–50.00 ng/mL for plasma with the limit of detection (LOD) of 0.030 ng/mL. The intra- and inter-day RSD were 5.51–8.63%, 2.28–9.95% and the RE was 0.18–1.65%. The recovery rates of letrozole and internal standard for plasma were 89.30–98.55%. Letrozole was stable under all the conditions in the study. The method was sensitive enough to quantitate letrozole over a period of 288 h after giving a single oral dose of 2.5 mg–24 Chinese healthy volunteers. The absorption of letrozole was rapid with small individual difference, the tissue distribution of letrozole was more than that in blood, and the clearance was slow. Letrozole was similar to three-compartment model in vivo. Due to metabolism and excretion, the AUCs of letrozole varied greatly among individuals.

Open access
Acta Chromatographica
Authors:
Chen Cheng
,
Nie Cun-Xi
,
Liang Jing
,
Wang Yong-Qiang
,
Liu Yan-Feng
,
Ge Wen-Xia
, and
Zhang Wen-Ju

A validated high-performance liquid chromatography (HPLC) method has been developed to analyze the (±)-gossypol in the selection of strains of Candida tropicalis culture. Since gossypol was easily degraded and oxidized, the addition of antioxidant NADPH-Na4 and acetone extraction was chosen to prevent gossypol degradation and gradient elution assay was applied to obtain gossypol resolution. Concentrations of gossypol in C. tropicalis ZD-3 culture 20 μg/mL were determined, and concentration–time profiles were observed. Linearity of the gossypol standard curve by HPLC area method was ranged from 0.1 to 20 μg/mL with Y = 26.954 × X − 29.547, R 2 = 0.9991, and n = 3, with limit of detection (LOD) of 50 ng/mL and lower limit of quantification (LLOQ) of 500 ng/mL. The recovery rate is dose-dependent and ranged from 85.3% to 103.5%. It is a rapid and reliable HPLC method for gossypol quantization in microorganism culture which could be applied in solid fermentation in the feed industry.

Open access
Journal of Behavioral Addictions
Authors:
Lu Li
,
Dan-Dan Xu
,
Jing-Xin Chai
,
Di Wang
,
Lin Li
,
Ling Zhang
,
Li Lu
,
Chee H. Ng
,
Gabor S. Ungvari
,
Song-Li Mei
, and
Yu-Tao Xiang

Background and aims

Internet addiction disorder (IAD) is common in university students. A number of studies have examined the prevalence of IAD in Chinese university students, but the results have been inconsistent. This is a meta-analysis of the prevalence of IAD and its associated factors in Chinese university students.

Methods

Both English (PubMed, PsycINFO, and Embase) and Chinese (Wan Fang Database and Chinese National Knowledge Infrastructure) databases were systematically and independently searched from their inception until January 16, 2017.

Results

Altogether 70 studies covering 122,454 university students were included in the meta-analysis. Using the random-effects model, the pooled overall prevalence of IAD was 11.3% (95% CI: 10.1%–12.5%). When using the 8-item Young Diagnostic Questionnaire, the 10-item modified Young Diagnostic Questionnaire, the 20-item Internet Addiction Test, and the 26-item Chen Internet Addiction Scale, the pooled prevalence of IAD was 8.4% (95% CI: 6.7%–10.4%), 9.3% (95% CI: 7.6%–11.4%), 11.2% (95% CI: 8.8%–14.3%), and 14.0% (95% CI: 10.6%–18.4%), respectively. Subgroup analyses revealed that the pooled prevalence of IAD was significantly associated with the measurement instrument (Q = 9.41, p = .024). Male gender, higher grade, and urban abode were also significantly associated with IAD. The prevalence of IAD was also higher in eastern and central of China than in its northern and western regions (10.7% vs. 8.1%, Q = 4.90, p = .027).

Conclusions

IAD is common among Chinese university students. Appropriate strategies for the prevention and treatment of IAD in this population need greater attention.

Open access