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Acta Chromatographica
Authors: Shanjiang Chen, Miaoling Huang, Zheng Yu, Jiamin He, Binge Huang, Xianqin Wang, Jianshe Ma, and Congcong Wen

8-O-Acetylharpagide is the main active component of the herb Ajuga decumbens, which possesses anti-tumor, anti-virus, and anti-inflammation properties. In this study, ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) was used to measure the concentration of 8-O-acetylharpagide in mouse blood, with subsequent investigation of the pharmacokinetics of the drug after intravenous or oral administration. Shanzhiside methyl ester was used as an internal standard, and the acetonitrile precipitation method was used to process the blood samples. Chromatographic separation was achieved using an ultra-performance liquid chromatography ethylene-bridged hybrid (UPLC BEH) column (2.1 mm × 50 mm, 1.7 μm) with a gradient methanol–water mobile phase (containing 0.1% formic acid). The flow rate was 0.4 mL/min, and the elution time was 5.0 min. 8-O-Acetylharpagide was quantitatively measured using electrospray ionization (ESI) tandem mass spectrometry in multiple reaction monitoring (MRM) mode with positive ionization. The result indicated that, within the range of 5–500 ng/mL, the linearity of 8-O-acetylharpagide in mouse blood was satisfactory (r > 0.995), and the lower limit of quantification (LLOQ) was 5 ng/mL. Intra-day precision relative standard deviation (RSD) of 8-O-acetylharpagide in blood was lower than 9%, and the inter-day precision RSD was lower than 13%. The accuracy range was between 94.3% and 107.1%, average recovery was higher than 91.3%, and the matrix effect was between 100.8% and 110.8%. This analytical method was sensitive and fast with good selectivity and was successfully applied to perform pharmacokinetic studies of 8-O-acetylharpagide in mice. The bioavailability of 8-O-acetylharpagide was 10.8%, and the analysis of the primary pharmacokinetic parameters after oral and intravenous administration indicated that 8-O-acetylharpagide had a significant first pass effect after oral administration.

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
Acta Chromatographica
Authors: Lianguo Chen, Qingwei Zhang, Yijing Lin, Xiaojie Lu, Zuoquan Zhong, Jianshe Ma, Congcong Wen, and Cheng Ding

An ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was established to determine the hapepunine in mouse blood, and the pharmacokinetics of hapepunine after intravenous (1.0 mg/kg) and intragastric (2.5, 5, and 10 mg/kg) administrations was studied. Delavinone was used as an internal standard. The UPLC ethylene bridged hybrid (BEH) C18 column was used for chromatographic separation. The mobile phase consisted of acetonitrile and 0.1% formic acid with a gradient elution flow rate of 0.4 mL/min. Multiple reaction monitoring (MRM) mode was used for quantitative analysis of hapepunine in electrospray ionization (ESI) positive interface. Proteins from mouse blood were removed by acetonitrile precipitation. The verification method was established in accordance with the US Food and Drug Administration (FDA) bioanalytical method validation guidelines. In the concentration range of 1–1000 ng/mL, the hapepunine in the mouse blood was linear (r 2 > 0.995), and the lower limit of quantification was 1.0 ng/mL. In the mouse blood, the intra-day precision coefficient of variation (CV) was less than 12%, the inter-day precision CV was less than 14%. The accuracy ranged from 91.7% to 109.3%. The average recovery was higher than 76.7%, and the matrix effect was between 86.0% and 106.4%. The UPLC–MS/MS method was sensitive, rapid, and selective and was successfully applied to the pharmacokinetic study of hapepunine in mice. The absolute bioavailability of hapepunine was 22.0%.

Open access

Hair is a stable specimen and has a longer detection window (from weeks to months) than blood and urine. Through the analysis of hair, the long-term information of the drug use of the identified person could be explored. Our work is to establish an ultra-performance liquid chromatography–tandem mass spectroscopy (UPLC–MS/MS) method for simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyamphetamine (MDA) in hair. Methoxyphenamine was used as an internal standard. The chromatographic separation was performed on a UPLC ethylene bridged hybrid (BEH) C18 (2.1 mm × 50 mm, 1.7 μm) column using a mobile phase of acetonitrile–water with 10 mmol/L ammonium acetate solution which containing 0.05% ammonium hydroxide. The multiple reaction monitoring in positive electrospray ionization was used for quantitative determination. The intra-day and inter-day precisions (relative standard deviation [RSD]) were below 15%. The accuracy ranged between 85.5% and 110.4%, the average recovery rate was above 72.9%, and the matrix effect ranged between 92.7% and 109.2%. Standard curves were in the range of 0.05–5.0 ng/mg, and the correlation coefficients were greater than 0.995. The established UPLC–MS/MS method was applied to analyze the hair samples successfully.

Open access
Acta Chromatographica
Authors: Aixia Han, Guanyang Lin, Jinzhang Cai, Qing Wu, Peiwu Geng, Jianshe Ma, Xianqin Wang, and Chongliang Lin

An ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was established to determine hirsutine and hirsuteine in rat plasma. Pharmacokinetics of hirsutine and hirsuteine in rats after intravenous or oral administration has been investigated using this developed UPLC–MS/MS method, and bioavailability of the two drugs was calculated. Diazepam was used as internal standard, and UPLC BEH column (2.1 mm × 50 mm, 1.7 μm) was used at temperature of 40 °C. The mobile phase was composed of acetonitrile and water (containing 0.1% formic acid) at a gradient elution flow rate of 0.4 mL/min. Nitrogen was used as desolvation gas (800 L/h) and conical gas (50 L/h). The multiple reaction monitoring (MRM) model was applied to quantitatively analyze hirsutine m/z 369 → 226, hirsuteine m/z 367 → 169.9, and diazepam (internal standard) m/z 285.1 → 193.3. Rat plasma samples were deproteinized using acetonitrile prior to UPLC–MS/MS analysis. Within the concentration range of 1–200 ng/mL, the linearity of hirsutine and hirsuteine in plasma was good (r > 0.995), and the lower limit of quantitation was 1 ng/mL. Relative standard deviations of intra-day precision for hirsutine and hirsuteine were ≤6.1% and ≤5.9%, respectively, and those of inter-day precision were ≤6% and ≤7.7%. Accuracy for hirsutine and hirsuteine ranged between 92.3% and 104.8%. Bioavailability of hirsutine and hirsuteine was 4.4% and 8.2%, respectively. The method is sensitive and fast with good selectivity and was successfully applied in the pharmacokinetic studies after intravenous and oral administration of hirsutine and hirsuteine.

Open access

Abstract

Liensinine is a bisbenzyltetrahydroisoquinoline alkaloid extracted from lotus (Nelumbo nucifera GAERTNER., Nelumbonaceae), especially in its embryo loti “Lien Tze Hsin” (green embryo of mature seed). A rapid and simple UPLC-MS/MS method was developed to determine liensinine in mouse blood and its application to a pharmacokinetic study. The blood samples were preprocessed by protein precipitation using acetonitrile. Midazolam (internal standard, IS) and liensinine were gradient eluted by mobile phase of methanol and water (0.1% formic acid) in a Waters UPLC BEH C18 column. The multiple reaction monitoring of m/z 611.3 → 206.1 for liensinine and m/z 326.2 → 291.1 for IS with an electrospray ionization (ESI) source was used for quantitative detection. The calibration curve ranged from 0.5 to 400 ng/mL (r > 0.995). The accuracy ranged from 92.2 to 108.2%, the precision of intra-day and inter-day was less than 14%, and the matrix effect was between 100.0% and 109.6%, the recovery was better than 71.0%. The developed UPLC-MS/MS method was successfully used for a pharmacokinetic study of liensinine in mice after oral (5 mg/kg) and intravenous administration (1 mg/kg), and the absolute availability of liensinine was 1.8%.

Open access
Acta Chromatographica
Authors: Ruijie Chen, Mengrou Lu, Xiaoting Tu, Wei Sun, Weijian Ye, Jianshe Ma, Congcong Wen, Xianqin Wang, and Peiwu Geng

We developed an ultra-performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS) method for quantification of panasenoside pharmacokinetics in rat plasma and tissue distribution in mouse. Twelve male Sprague-Dawley rats were used for pharmacokinetics after intravenous (2 or 10 mg/kg) administration of panasenoside, six rats for each dose. Thirty mice were randomly divided into six groups (five mice for each group, one group for each time point) and received 20 mg/kg of panasenoside by intraperitoneal administration. Calibration plots were in the range of 2–2000 ng/mL for panasenoside in rat plasma and 2–3000 ng/mL in mouse tissues. The relative standard deviation (RSD) of inter-day and intra-day precision was less than 14%. The accuracy was between 89.6% and 110.0%. The AUC(0–t) was 160.8 ± 13.0 and 404.9 ± 78.0 ng/mL*h, and t 1/2 of 3.2 ± 1.2 and 4.6 ± 1.7 h, CL (clearance) of 10.0 ± 2.0, and 21.4 ± 2.0 L/h/kg after intravenous administration 2 mg/kg and 10 mg/kg of panasenoside, respectively. The tissue distribution results indicated that the panasenoside diffuses rapidly and widely into major organs. The level of panasenoside was highest in mouse liver, followed by kidney, lung, and spleen. The overwhelming accumulation in liver indicated that liver was responsible for the extensive metabolism.

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 Cmax 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

Carbofuran is a carbamate pesticide, a broad-spectrum, high-efficiency, low-residue, and highly toxic insecticide, acaricide, and nematicide, widely used in agriculture. Carbofuran is most harmful to birds, and birds or insects killed by furan poisoning can be killed by secondary poisoning after being foraged by raptors, small mammals, or reptiles. In this paper, an UPLC-MS/MS method was developed for the determination of carbofuran and its metabolite, 3-hydroxycarbofuran, in duck liver. Liver tissue was first ground into a homogenate and then passed through ethyl acetate liquid-liquid extraction processing samples. Multiple reaction monitoring (MRM) mode was used for quantitative analysis, m/z 222.1 → 165.1 for carbofuran, m/z 238.1 → 180.9 for 3-hydroxycarbofuran and m/z 290.2 → 198.2 for an internal standard. The standard curves of carbofuran and 3-hydroxycarbofuran in duck liver were within a range of 2–2000 ng/g, where the linearity was good, the lower limit of quantification was 2 ng/g. The intra-day precision of carbofuran and 3-hydroxycarbofuran was <14%, and the inter-day precision was <13%, the accuracy range was between 91.8 and 108.9%, the average extraction efficiency was higher than 75.1% with a matrix effect between 93.4 and 107.7%. The developed method was applied to a situation of suspected duck poisoning at a local farm.

Open access