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Validated LC-MS/MS method for quantitation of solasodine in rat urine and feces: Blocking nonspecific adsorption

Lu Tiantian, Wang Xiaohong, Zhang Qi, Liu Kun, Xu Tongxin, Wang Quande, Zhao Pengfei, Cheng Zhongzhe

Acta Chromatographica

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2023

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Vol. 35, no. 4

319--325

EN

Solasodine, a steroidal alkaloid, is distributed extensively in Solanaceae plants with multiple biological activities such as neuroprotection, antineoplastic and anticonvulsant activities. However, there is little information about the excretion of intact solasodine in vivo. To investigate its excretion, a reliable LC-MS/MS method for quantitation solasodine in rat urine and feces was established and validated. Sample preparation was carried out by liquid-liquid extraction using MTBE as extractant. Moreover, rat urine was preconditioned with BSA, an anti-adsorptive additive, to prevent the nonspecific binding of solasodine to containers and tubes. The method was validated over the range of 4–2000 ng mL⁻¹. The correlation coefficient (r2t) were all above 0.999. The intra- and inter-day precision and accuracy were within 16.9% and between −11.0 and 8.9%, respectively. The recovery of solasodine in urine and feces was in the range of 72.5–80.3 and 75.7–80.2%, respectively. IS-normalized matrix factor ranged from 0.94 to 1.12 with RSD% ≤4.02%. This method was successfully applied to the excretion study of solasodine following oral and intravenous administration.

2

Study on pharmacokinetics, tissue distribution, and excretion of phloretin and its prodrug 2′,4′,6′,4-Tetra-O-acetylphloretin in rats using LC–MS/MS

Wang Libin, Li Xi, Mi Le, Shen Xin, Feng Tian, Liu Xueying, Wang Qingwei

Acta Chromatographica

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2019

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Vol. 31, no. 1

63--70

EN

2′,4′,6′,4-Tetra-O-acetylphloretin (TAPHL) is a prodrug of phloretin (PHL) in which the OH groups are protected by acetylation. A validated liquid chromatography–tandem mass spectrometry (LC–MS/MS) method for the determination of PHL in rat biological matrices was developed and applied to investigate and compare the pharmacokinetics, tissue distribution, and excretion of PHL and TAPHL in rats following a single oral administration. The method was validated for accuracy, precision, linearity, range, selectivity, lower limit of quantification (LLOQ), recovery, and matrix effect. All validation parameters met the acceptance criteria according to regulatory guidelines. The mean pharmacokinetic parameters of tmax, Cmax, AUC(0 − t), CL/F, and t1/2 were observed after oral administration in rats. The data showed that PHL was absorbed and eliminated rapidly from plasma after oral administration. The pharmacokinetic properties are improved, such as the tmax has been prolonged and the area under the curve (AUC) has been enhanced after oral administration of TAPHL to rats. Tissue distribution results indicated that PHL could be rapidly and widely distributed into tissues but could not effectively cross the blood–brain barrier in rats. After oral administration of TAPHL to rats, its tissue distribution to rats was similar as that after oral administration of equimolar PHL. In addition, higher recoveries of PHL following administration of TAPHL indicated that TAPHL might reduce the excretion of PHL from the body by reducing the first pass effect.

3

Excretion study of 10-Methoxycamptothecin and its metabolite 10-Hydroxycamptothecin in rats by RP-HPLC method with fluorescence detection

Changmin S., Zheng J., Chi J., Jing L., Xiufeng Y., Wang Y.

Acta Chromatographica

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2017

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Vol. 29, no. 4

453--458

EN

10-Methoxycamptothecin (MCPT) and 10-hydroxycamptothecin (HCPT) are the indole alkaloids isolated from a Chinese tree, Camptotheca acuminata, and have a wide spectrum of anticancer activity in vitro and in vivo mainly through inhibitory effects on topoisomerase I. HCPT is a major metabolite of MCPT in rats; the pharmacokinetic analysis and tissue distribution of MCPT and HCPT in rats have also been determined after i.v. injection of MCPT, but the excretion of MCPT and its metabolite HCPT has not been assessed up to now. In the present study, the excretion study of MCPT and its metabolite HCPT in rat bile, feces, and urine after i.v. administration of MCPT (5 mg kg-1) was performed by high performance liquid chromatography (HPLC) method coupled with a fluorescence detector. The results showed that MCPT mainly biotransformed to HCPT and excreted in the form of HCPT and MCPT in bile, urine, and feces after i.v. administration of MCPT. It was excreted about 1.24 ± 0.07% as MCPT and 5.49 ± 0.40% as HCPT in bile within 6 h after i.v. administration. The cumulative excretions of MCPT and HCPT were mainly within 24 h after i.v. administration, which were 0.41 ± 0.10% and 7.66 ± 1.43% of the dosage in urine and about 0.16 ± 0.04% and 20.30 ± 3.35% of the dosage in feces. The total excretion of MCPT in urine, bile, and feces was 1.81 ± 0.09% in the form of original MCPT and 33.45 ± 1.57%. detected as the metabolite HCPT in urine, bile, and feces, suggesting that MCPT might undergo other biotransformation.

4

Simultaneous determination and excretion study of six flavonoids in rat after oral administration of Fructus Sophorae extract by liquid chromatography tandem mass spectrometry

Zhi X. R., Zhang Z. Y., Li R. Y., Chang L., Jia P. P., Sheng N., Zhang L. T.

Acta Chromatographica

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2016

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Vol. 28, no. 1

33--50

EN

A new, sensitive, and selective high-performance liquid chromatography-tandem mass spectrometric method (HPLC-MS/MS) has been developed for the quantification of six flavonoids (sophoricoside, genistin, genistein, rutin, quercetin, and kaempferol) in rat bile and urine. The sample pretreatment was simple by liquid-liquid extraction. Sulfamethalazole was used as internal standard (IS). During method development, the effect of extraction volume, mobile phase composition, column temperature, and injection volume were varied to optimize sensitivity and achieve a run time as short as possible. Chromatographic separation was accomplished on a C18 column with a simple linear gradient elution within 9 min. Full validation of the assay was in accordance with the requirement of the validation of the method in vivo and implemented including specificity, linearity, accuracy, precision, recovery, and matrix effect. This is the first report on determination of the major flavones in rat bile and urine after oral administration of Fructus Sophorae extract. The method has been used successfully in excretion studies of six major flavonoids in rat bile and urine.

5

Simultaneous and sensitive determination of eight coumarins in rat bile and urine after oral administration of Radix Angelicae Dahuricae extract by liquid chromatography-electrospray ionization-mass spectrometry

Huo H. L., Yu S. H., Liu X. Z., Meng Y., Ren Y. P., Zhang L. T.

Acta Chromatographica

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2013

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Vol. 25, no. 2

201--219

EN

A selective and sensitive liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) method was developed and validated for analysis of xanthotoxol (1), xanthotoxin (2), isoimpinellin (3), bergapten (4), oxypeucedanin (5), imperatorin (6), cnidilin (7), and isoimperatorin (8) in rat bile and urine using pimpinellin as an internal standard (IS). An Agilent 1200 liquid chromatography system (Agilent Technologies, USA) equipped with a quaternary pump, an autosampler, and a column compartment was used for all analyses. Chromatographic separations were performed on a Sapphire C18 column (150 mm × 4.6 mm, 5 μm), and the column temperature was maintained at 30°C; the sample injection volume was 10 μL. The specificity, linearity, accuracy, precision, recovery, matrix effect, and several stabilities were validated for all analytes in the rat bile and urine samples. The method was successfully applied in monitoring the concentrations of eight coumarins in rat bile and urine after a single oral administration of Radix Angelicae Dahuricae extract with a dosage of 8.0 mL/kg. In the bile samples, the eight coumarins excreted completely in twenty-four hours. The average percentages of coumarins (1–8) excreted were 0.045%, 0.019%, 0.177%, 0.105%, 0.337%, 0.023%, 0.024%, 0.021%. In the urine samples, the eight coumarins excreted completely in seventy-two hours. The average percentages of coumarins (1–8) excreted were 1.78%, 0.095%, 0.130%, 0.292%, 0.082%, 0.008%, 0.005%, 0.004%. The method is robust and specific and it can successfully complete the requirements of the excretion study of the eight coumarins in Radix Angelicae Dahuricae.

6

Accumulation of polonium by Mytilus trossulus under experimental conditions

Stepnowski P., Kożuch J.

Oceanological Studies

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1999

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Vol. 28, No. 1-2

73-82

EN

The bioaccumulation of polonium in the Baltic mussel Mytilus trossulus was studied experi-mentally in an attempt to discover the differences between food and water as sources of polonium. The 209Po isotope was used as tracer for accumulation and excretion. The highest 209Po con-centration was found in the hepatopancreas of mussels exposed to spiked water for 24 days. Both parts of the experiment (exposure to food and water) showed that while the rate of bioaccumula-tion of polonium by Mytilus trossulus was very high, the excretion rate was also relatively high. Furthermore, in both cases the duration of the accumulation-excretion (a-e) cycle of polonium in Mytilus trossulus was 10 days. Finally, a simple mathematical model approximating the experimental data was developed.