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1

Simultaneous determination of ginkgolide A, B, C, bilobalide and rutin in rat plasma by LC-MS/MS and its application to a pharmacokinetic study

Hu Bingying, Sun Yingying, Wang Min, He Zhisheng, Chen Shanshan, Qi Dake, Ge Zhen, Fan Lingling, Chen Jingfang, Wei Yang

Acta Chromatographica

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2022

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Vol. 34, no. 4

386--393

EN

A reliable LC-MS/MS method for the determination of five bioactive constituents (bilobalide, BLL; ginkgolide A, GLA; ginkgolide B, GLB; ginkgolide C, GLC; rutin) of Ginkgo biloba leaf extracts (GBE) in rat plasma was established, fully validated and applied to an intragastric pharmacokinetic study of a preparation of GBE in rat. Samples were extracted with ethyl acetate. C18 column was selected as analytical column in this method. Mobile phase was water with 0.01% formic acid and acetonitrile. Quantification was performed in negative multiple-reaction monitoring mode. Matrix instability of terpene lactones was noticed and hydrochloric acid was used as a stabilizer. This method showed good precision and accuracy, recovery was reproducible and matrix effect was negligible. Among four terpene lactones, BLL had the highest exposure and the shortest terminal half-life, GLA and GLB had lower exposure and longer terminal half-life, the exposure of GLC was lowest and its terminal half-life was the maximum, and all of them showed rapid absorption. This study provides a reference for determination of terpene lactones and flavonol glycoside prototypes in GBE and offers pharmacokinetic data of flavonol glycoside prototype in GBE.

2

LC-MS/MS determination of glimepiride in human plasma with a high recovery at picogram scale : pharmacokinetic study after oral administration

Kammoun Ahmed K., Awan Zuhier Ahmed, Elawady Tarek, Khedr Alaa, El-Awady Mohamed I.

Acta Chromatographica

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2022

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Vol. 34, no. 1

12--17

EN

Although glimepiride (GLM) is the first-line treatment of Type II diabetes, low extraction recovery is still a significant limitation in previous plasma analysis methods. An optimized solid-phase extraction method of GLM in human plasma with excellent extraction recovery, 100 ± 0.06%, was achieved using liquid chromatography-electrospray ionization tandem mass spectrometry and Gliclazide (GLZ) as an internal standard. GLM was extracted from 100 µL plasma sample using Sep-Pak® vac 1cc (100 mg) C18 column and methylene chloride: methanol (2: 1, v/v) as eluant. Both GLM and GLZ were monitored by a triple quad mass spectrometer applying positive multiple reaction monitoring mode (+MRM). The protonated precursor ions and product ions of GLM and GLZ were m/z 491(352), and m/z 324 (127), respectively. The detection and measurement of low levels of GLM in human plasma reached to picogram range (limit of detection (LOD) = 60 pg/mL, limit of quantification (LOQ) = 200 pg/mL). The method was validated in terms of selectivity, linearity, recovery, accuracy, and precision. The method was successfully applied to the pharmacokinetic study of GLM following oral administration of 1 mg GLM tablets to 12 healthy volunteers.

3

Effect of Citrus suavissima Hort. ex Tanaka on pharmacokinetics of erlotinib in rat plasma by UPLC-MS/MS

Yang Jinzhao, Liu Huamin, Cai Yuan, Wu Yazhen, Xu Xiaoxin, Wang Xianqin, Lin Chongliang

Acta Chromatographica

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2021

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Vol. 33, no. 1

73--77

EN

Twelve Sprague-Dawley rats were randomly divided into two groups: Citrus suavissima Hort. ex Tanaka group and control group (n 5 6). The rats in Citrus suavissima Hort. ex Tanaka group were given Citrus suavissima Hort. ex Tanaka juices (1 mL/100 g) by oral administration each day, continued for 14 days; the rats in control group were given Stroke-physiological saline solution (1 mL/100 g) by oral administration each day, continued for 14 days. The rats of these two groups were given a single oral administration of erlotinib (20 mg/kg) on the 15th day. After blood sampling at different time points and processing, the concentrations of erlotinib in rat plasma were determined by the established ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method. Chromatographic separation was achieved using a UPLC BEH C18 column (2.1 mm 3 50 mm, 1.7 mm) with erlotinib-d6 as an internal standard (IS). The initial mobile phase consisted of acetonitrile and water (containing 0.1% formic acid) with gradient elution. Multiple reaction monitoring (MRM) modes were utilized to conduct quantitative analysis. The sensitive, rapid and selective UPLC-MS/MS method was successfully applied to analyse the effect of Citrus suavissima Hort. ex Tanaka on pharmacokinetics of erlotinib in rat plasma. There were no significant differences in AUC(0t), t1/2, Tmax, CL, Cmax between the two groups (P > 0.05). While MRT(0t) was decreased (P < 0.05) in Citrus suavissima Hort. ex Tanaka group, compared to the control group. It showed that Citrus suavissima Hort. ex Tanaka could not affect the metabolism of erlotinib.

4

Pharmacokinetic UPLC–MS/MS studies on byakangelicol after oral and intravenous administration to rats

Bao Xi, Huang Bingee, Mao Yiting, Zhang Zhiguang, Zhou Yunfang, Wen Congcong, Zhou Quan

Acta Chromatographica

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2020

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Vol. 32, no. 1

49--52

EN

Byakangelicol is one of coumarins from Baizhi and has been shown to inhibit the release of PGE2 from human lung epithelial A549 cells in a dose-dependent manner. A sensitive ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed and full validated for the quantification of byakangelicol in rat plasma. The pharmacokinetics of byakangelicol after both intravenous (5 mg/kg) and oral (15 mg/kg) administrations were studied. Chromatographic separation was performed on an ultra-performance liquid chromatography ethylene bridged hybrid (UPLC BEH) C18 column with acetonitrile and 0.1% formic acid as the mobile phase at a flow rate of 0.4 mL/min; fargesin was used as the internal standard (IS). The following quantitative analysis of byakangelicol was utilized in the multiple reaction monitoring mode. The samples were extracted from rat plasma via protein precipitation using acetonitrile. In the concentration range of 1–2000 ng/mL, the method correlated linearity (r > 0.995) with a lower limit of quantitation (LLOQ) of 1 ng/mL. Intra-day precision was less than 11%, and inter-day precision was less than 12%. The accuracy was between 92.0% and 108.7%, the recovery was better than 89.6%, and the matrix effect was between 85.9% and 98.6%. The method was successfully applied to a pharmacokinetic study of byakangelicol after intravenous and oral administration, and the absolute bioavailability was 3.6%.

5

Development and validation of high-performance liquid chromatographic method for quantification of Irinotecan and its active metabolite SN-38 in colon tumor bearing NOD/SCID mice plasma samples: application to pharmacokinetic study

Taneja Neetika, Gota Vikram, Gurjar Murari, Singh Kamalinder K.

Acta Chromatographica

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2019

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Vol. 31, no. 3

166--172

EN

Irinotecan (IRT) is an antineoplastic agent widely used in the treatment of various cancers primarily in colorectal cancer. A new, simple and sensitive high-performance liquid chromatography (HPLC) method coupled with fluorescence detector was developed and validated to quantify IRT and its active metabolite SN38 in the plasma of non-obese diabetic/severe combined immune-deficient mice (NOD/SCID) mice bearing colon tumor. The plasma samples were extracted by precipitation method using acetonitrile with 0.1% formic acid. The chromatographic separation was achieved using mobile phase consisted of water and acetonitrile (57:43 v/v) pH 3 at the flow rate of 0.8 mL/min in C18 column (internal diameter, 250 × 4.6 mm; pore size, 5 μm). The method was validated according to the bioanalytical guidelines defined by Food and Drug Administration (FDA) and European Medicine Agency (EMA). A regression (R2) value of 0.999 and 0.997 for IRT and SN38 suggested the good linearity in the range of 0.1–10 μg/mL and 5–500 ng/mL, respectively. The calculated lower limit of quantification (LLOQ) and limit of detection (LOD) for IRT were 0.1 and 0.065 μg/mL, respectively. However, for SN38, LLOQ and LOD were 5 and 2 ng/mL, respectively. The intra-day and inter-day variations (coefficient of variance; % CV) observed during the validation were found to be within the set limit of 15%. Both accuracy and percentage recovery analyzed and calculated from the quality control samples were in the between the defined range of 85–115%. Plasma samples were found to be stable when stored at room temperature for 2 h, after 2 freeze–thaw cycles and at −80 °C for 2 months. The developed method was successfully applied to study the plasma elimination profile of IRT in NOD/SCID mice with tumor. The results from plasma concentration time profile and pharmacokinetic parameter analyzed suggested the rapid elimination of IRT and SN38 from the plasma of NOD/SCID mice.

6

Sterowanie selektywnością w badaniach farmakokinetycznych

Musijowski J., Gilant E., Rudzki P. J.

Przemysł Chemiczny

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2012

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T. 91, nr 3

381-386

PL

Sterowanie selektywnością jest procesem leżącym w zakresie optymalizacji metody bioanalitycznej. Praca zawiera podstawowe informacje na temat czynników chemicznych i instrumentalnych, na różnych etapach postępowania analitycznego, mających znaczący wpływ na selektywność metod stosowanych w badaniach farmakokinetycznych. Ze względu na obszerność tematyki, w pracy skoncentrowano się przede wszystkim na kontroli selektywności w zakresie metod przygotowania próbki, niektórych technik rozdzielania oraz wybranych detektorów.

EN

A review, with 28 refs., of methods for isolation, sepn. and detection of drug active ingredients from biolog. material.

7

Simultaneous determination of nine flavonoids in beagle dog by HPLC with DAD and application of Ginkgo biloba extracts on the pharmacokinetic

Wu J., Xing H, Tang D., Gao Y., Yin X, Du Q., Jiang X., Yang D.

Acta Chromatographica

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2012

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Vol. 24, no. 4

627--642

EN

The method of high-performance liquid chromatography (HPLC) with diode array detector (DAD) was used and validated for the simultaneous determination of nine flavonoids (rutin, myricetin, quercitrin, quercetin, luteolin, genistein, kaempferol, apigenin, and isorhamnetin) in beagle dog plasma. Plasma sample was pre-treated with acetonitrile (containing 0.05% formic acid). Chromatographic separation was performed on a kromasil C18 column (250 × 4.6 mm, 5 µm) maintained at 35 °C. The mobile phase was a mixture of methanol and 0.2% formic acid with a step linear gradient. At 1.0 mL min-1 flow rate, the eluent of other eight flavonoids was detected simultaneously at 360 nm with good separation except genistein (detected at 254 nm). Under optimum conditions, the correlation coefficient between the peak area and the concentrations for each analyte was all above 0.999. The intra-day and inter-day precisions were less than 10% for all analytes. The limit of detection and the limit of quantification for the selected nine flavonoids were 0.006–0.03 and 0.02–0.12 g mL, -1 respectively. The extracted recoveries of selected nine flavonoids were 74.02%–99.37%. The assay has been successfully applied to determine concentrations of nine flavonoids in plasma from beagle dog after being intravenously administrated Ginkgo biloba extract.

8

Method development and validation of an HPLC assay for the detection of hopantenic acid in human plasma and its application to a pharmacokinetic study on volunteers

Pozharitskaya O. N, Kosman V. M, Karlina M. V, Shikov A. N, Makarov V. G, Djachuk G. I

Acta Chromatographica

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2011

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Vol. 23, no. 3

403--414

EN

A reliable and sensitive reversed-phase high performance liquid chromatography (RP-HPLC) with ultraviolet (UV) detection method was developed and validated for the quantification of hopantenic acid in human plasma. Hopantenic acid, with protocatechuic acid as the internal standard (IS), was extracted from plasma samples using a liquid-liquid extraction with methanol. A chromatographic separation was achieved on a Luna C18 column (4.6 mm × 150 mm, 5-μm particle size) and precolumn of the same sorbent (2.0 mm). An isocratic elution, at a flow rate of 1.0 mL min -1, was used with a mobile phase consisting of acetonitrile, water, and 0.03% trifluoroacetic acid. The UV detector was set to 205 nm. The elution times for hopantenic acid and IS were ∼4.3 and 5.4 min, respectively. The calibration curve of hopantenic acid was linear (r > 0.9994) over the range of 0.5–100 μg mL−1 in human plasma. The limit of detection and limit of quantification for hopantenic acid were 0.034 and 0.103 μg mL -1, respectively. The present method was successfully applied for the estimation of pharmacokinetic parameters of hopantenic acid following single oral administration of tablets containing 250 mg hopantenic acid to healthy volunteers. For hopantenic acid, the data showed a mean maximum plasma concentration (Cmax) of 2.32 μg mL, -1 with a time to reach peak plasma concentration (tmax) of 1.56 h.