High-performance liquid chromatographic assay for α-lipoic acid and five of its metabolites in human plasma and urine

Teichert, Jens; Preiss, R

doi:10.1016/s1570-0232(02)00010-7

Cited by 52 publications

(48 citation statements)

References 7 publications

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“…The LODs and LOQs for the two analytes are given in Table 3, showing that the proposed method was more sensitive than the previously reported methods for simultaneous determination of the two analytes that have detection limits of 1 and 5 ng mL -1 for a-LA and DHLA, respectively [12,15,17,20,26], and could be used to determine the endogenous level of the free forms of the analytes in the intended biological matrices. Sensitivity of the two analytes can be further increased by increasing the injection volume.…”

Section: Sensitivitymentioning

confidence: 92%

“…Other disadvantages of the LLE methods over PP methods are that these procedures are multi-step, laborious, and time consuming. Solidphase extraction (SPE) procedures have also been reported for the extraction of the a-LA from complex sample matrices [12,13,15,17,20], and these procedures offer comparable recoveries and clear chromatograms. However, SPE is a much more expensive procedure than the LLE and PP, so it was not utilized in this study.…”

Section: Optimization Of Sample Preparationmentioning

confidence: 99%

“…Several papers have been published on the chromatographic analysis of total, free, or bound a-LA in various sample matrices such as foodstuffs [9], dietary supplements [10], and biological samples [11][12][13][14][15][16]. Similarly, very few methods [17][18][19][20][21][22][23] are available for simultaneous determination of the total a-LA and its reduced form, DHLA, in biological samples after oral administration.…”

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confidence: 99%

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Simultaneous Determination of the Endogenous Free α-Lipoic Acid and Dihydrolipoic Acid in Human Plasma and Erythrocytes by RP-HPLC with Electrochemical Detection

et al. 2011

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A highly sensitive, precise, and accurate reversed-phase high-performance liquid-chromatography/ electrochemical detection method for simultaneous determination of the endogenous free a-lipoic acid and dihydrolipoic acid in biological matrices was developed and validated. The two analytes were extracted from the samples with acetonitrile/10% metaphosphoric acid solution (aqueous) (50/50 v/v). To determine the total lipoic acid, samples were treated with tris(2-carboxyethyl)phosphine solution in phosphate buffer, pH 2.5 with 85% orthophosphoric acid prior to deproteination. The two analytes were separated on a C 18 (150 9 4.6 mm, 5 lm) analytical column using acetonitrile-50 mM phosphate buffer, pH 2.5 with 85% orthophosphoric acid (35/65 v/v) as the isocratic mobile phase pumped at a flow rate of 2.0 mL min -1 at the column oven temperature of 35°C. The column eluents were monitored at a potential of 0.9 V. These analytes were efficiently resolved in \7 min. The present method was sufficiently robust and specific for simultaneous determination of the two analytes and demonstrated acceptable values for linearity (r 2 = 0.999 in the range of 0.1-500 and 0.25-1,000 ng mL -1 for a-lipoic acid and dihydrolipoic acid, respectively), recovery ([97%), precision (RSD% \2), and sensitivity (on column limit of detection, 150 and 375 fg for a-lipoic acid and dihydrolipoic acid, respectively and limit of quantification: 0.5 and 1.25 pg for a-lipoic acid and dihydrolipoic acid, respectively), indicating that the proposed method was more sensitive, precise, economical, and versatile, and has higher throughput than the previously reported methods for simultaneous determination of the two analytes.

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Section: Sensitivitymentioning

confidence: 92%

Section: Optimization Of Sample Preparationmentioning

confidence: 99%

mentioning

confidence: 99%

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Simultaneous Determination of the Endogenous Free α-Lipoic Acid and Dihydrolipoic Acid in Human Plasma and Erythrocytes by RP-HPLC with Electrochemical Detection

et al. 2011

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“…It is concentrated to the highest levels in the liver and only minor amounts from food or biosynthesis enter the blood circulation [Nichols, 1997]. In particular, the plasma half-life of a-lipoic acid is less than 1 h, after which it is excreted, mainly in the urine, within 24 h [Hermann et al, 1996;Teichert and Preis, 2002].…”

Section: Biochemical Transformations Involving Mitochondriamentioning

confidence: 99%

Lactic acid in cancer and mitochondrial disease

Steliou

Perrine

Faller

2009

Drug Development Research

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Cancer and the mitochondrial diseases are disparate disorders that have in common a failure of normal cellular respiratory activity in disease-affected tissues. In mitochondrial diseases, the impairment in the mitochondria is often the result of abnormalities in their mtDNA, whereas in cancerous cells, the altered respiration is driven by the Warburg effect. The oxidation of glucose (as pyruvate in the mitochondria) is inhibited and energy production relies on cytoplasmic glycolysis. This suppressed mitochondrial activity confers in tumor cells a state of resistance to apoptosis and, in mitochondrial diseases like mitochondrial encephalopathy, lactic acidosis, and stroke-like episodes (MELAS), the altered respiration leads to lactic acidosis. Driving glucose to its complete oxidation inside the mitochondria has potential in cancer therapy to reconstitute apoptotic competence in tumor cells and, in mitochondrial disease, to treat lactic acidosis. This minireview investigates the development of small molecule agents for suppressing the Warburg effect in cancer therapy and lactic acidosis in mitochondrial disease. Drug Dev Res 70 : 499-511, 2009.

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“…Owing to the recent reports involving metabolism of lipoic acid (Teichert and Preiss, 2002;Schupke et al, 2002), it becomes clear that plasma lipoic acid levels are considerably low and perhaps variable. Therefore, a sensitive, simple and reproducible bioanalytical method is important in investigating the pre-clinical and clinical pharmacokinetic studies and relevant drug-drug interaction and bioequivalence studies of lipoic acid.…”

Section: Introductionmentioning

confidence: 99%

Determination of lipoic acid in rat plasma by LC‐MS/MS with electrospray ionization: Assay development, validation and application to a pharamcokinetic study

Trivedi¹,

Kallem²,

Mamidi³

et al. 2004

Biomedical Chromatography

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A simple, sensitive and specific LC-MS/MS method for the determination of lipoic acid was developed and validated over the linearity range 5-1000 ng/mL (r2 > 0.99) with 200 microL rat plasma using rosigliatzone as an internal standard (IS). The assay procedure involved a simple one-step liquid-liquid extraction of lipoic acid and IS from plasma into ethyl acetate. The organic layer was separated and evaporated under a gentle stream of nitrogen at 40 degrees C. The residue was reconstituted in the mobile phase and injected onto a Hichrom RPB column (4.6 x 250 mm, 5 microm). Separation of lipoic acid and IS was achieved with a mobile phase consisting of 0.05 M formic acid:acetonitrile (40:60, v/v) at a flow rate of 1.0 mL/min. The API-3000 LC-MS/MS was operated under the multiple reaction monitoring mode (MRM) using the electrospray ionization technique. Positive and negative ion acquisition within the same chromatographic run was used in the present method. For lipoic acid a pseudo-molecular ion transition pair was acquired in negative polarity, whereas for IS the transition pair was acquired in positive polarity. Quantitation was determined for both analyte and IS in MRM scan mode. Absolute recovery of lipoic acid and IS was >70 and 97%, respectively. The lower limit of quantification (LLOQ) of lipoic acid was 5.0 ng/mL. The inter- and intra-day precision in the measurement of quality control (QC) samples 5, 15, 400 and 800 ng/mL were in the range 2.18-5.99% relative standard deviation (RSD) and 0.93-13.77% RSD, respectively. Accuracy in the measurement of QC samples was in the range 87.40-114.40% of the nominal values. Analyte and IS were stable in the battery of stability studies, viz. bench-top, auto-sampler and freeze-thaw cycles. Stability of lipoic acid was established for 1 month at -80 degrees C. The application of the assay to a pharmacokinetic study in rats confirmed the utility of the assay.

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High-performance liquid chromatographic assay for α-lipoic acid and five of its metabolites in human plasma and urine

Cited by 52 publications

References 7 publications

Simultaneous Determination of the Endogenous Free α-Lipoic Acid and Dihydrolipoic Acid in Human Plasma and Erythrocytes by RP-HPLC with Electrochemical Detection

Simultaneous Determination of the Endogenous Free α-Lipoic Acid and Dihydrolipoic Acid in Human Plasma and Erythrocytes by RP-HPLC with Electrochemical Detection

Lactic acid in cancer and mitochondrial disease

Determination of lipoic acid in rat plasma by LC‐MS/MS with electrospray ionization: Assay development, validation and application to a pharamcokinetic study

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