Fast screening of lovastatin in red yeast rice products by flow injection tandem mass spectrometry

Song, Fenhong; El-Demerdash, Aref; Lee, Shwn-Ji Susie H.; Smith, Robert E.

doi:10.1016/j.jpba.2011.08.039

Cited by 27 publications

(23 citation statements)

References 15 publications

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“…An assay of seven main monacolins, monacolin K (lovastatin), monacolin J, monacolin L and their corresponding hydroxy acid forms and dehydromonacolin K, representing 97% of total monacolins, was determined. In order to shorten the analysis time Song et al proposed a fast screening method of lovastatin in red yeast rice products by flow injection tandem mass spectrometry without LC separation [16].…”

Section: Lovastatinmentioning

confidence: 99%

A Review of Current Trends and Advances in Analytical Methods for Determination of Statins: Chromatography and Capillary Electrophoresis

Nigović¹,

Mornar²,

Sertić³

2012

Chromatography - The Most Versatile Method of Chemical Analysis

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Section: Lovastatinmentioning

confidence: 99%

A Review of Current Trends and Advances in Analytical Methods for Determination of Statins: Chromatography and Capillary Electrophoresis

Nigović¹,

Mornar²,

Sertić³

2012

Chromatography - The Most Versatile Method of Chemical Analysis

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“…Previous analytical approaches mainly used high-performance liquid chromatography (HPLC) with diode array or mass spectrometric detectors [27-33]. Song et al [34] suggested a flow injection tandem mass spectrometry for screening analysis. Chromatographic and mass spectrometric methods have some problems in separating over 14 monacolins and avoiding co-eluting interferences that could cause overestimation of the quantities of the analytes [34].…”

Section: Introductionmentioning

confidence: 99%

“…Song et al [34] suggested a flow injection tandem mass spectrometry for screening analysis. Chromatographic and mass spectrometric methods have some problems in separating over 14 monacolins and avoiding co-eluting interferences that could cause overestimation of the quantities of the analytes [34]. Furthermore, an equilibrium exists between monacolin K and its lactone ring opened hydroxy acid form (ratio between 2:1 and 3:2), which can be chromatographically separated [32].…”

Section: Introductionmentioning

confidence: 99%

NMR evaluation of total statin content and HMG-CoA reductase inhibition in red yeast rice (Monascus spp.) food supplements

et al. 2012

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BackgroundRed yeast rice (i.e., rice fermented with Monascus spp.), as a food supplement, is claimed to be blood cholesterol-lowering. The red yeast rice constituent monacolin K, also known as lovastatin, is an inhibitor of the hydroxymethylglutaryl-CoA (HMG-CoA) reductase. This article aims to develop a sensitive nuclear magnetic resonance (NMR) method to determine the total statin content of red yeast rice products.MethodsThe total statin content was determined by a 400 MHz 1H NMR spectroscopic method, based on the integration of the multiplet at δ 5.37-5.32 ppm of a hydrogen at the hexahydronaphthalene moiety in comparison to an external calibration with lovastatin. The activity of HMG-CoA reductase was measured by a commercial spectrophotometric assay kit.ResultsThe NMR detection limit for total statins was 6 mg/L (equivalent to 0.3 mg/capsule, if two capsules are dissolved in 50 mL ethanol). The relative standard deviations were consistently lower than 11%. The total statin concentrations of five red yeast rice supplements were between 1.5 and 25.2 mg per specified daily dose. A dose-dependent inhibition of the HMG-CoA reductase enzyme activity by the red yeast rice products was demonstrated.ConclusionA simple and direct NMR assay was developed to determine the total statin content in red yeast rice. The assay can be applied for the determination of statin content for the regulatory control of red yeast rice products.

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“…Similar methods are now used in many nationwide neonatal screening programs [23,24]. In the fields of pesticide determination [25,26,27], therapeutic drug monitoring [28] and analysis of adulterated dietary supplements [29], FIA-MS/MS has recently been presented as an adequate alternative to LC-MS/MS. For FIA-MS/MS the mass spectrometer is directly coupled to a pump delivering a continuous flow of eluent solvents, whereas the LC column compartment is bypassed.…”

Section: Introductionmentioning

confidence: 99%

“…FIA-MS/MS in complex biological matrices like plasma or urine is typically done after straightforward sample dilution in organic solvents for precipitation of proteins and reduction of ion suppression effects, an approach known as ‘dilute and shoot’. The two most important analytical challenges of FIA-MS/MS are: (1) assessment and exclusion of coelution bias, which is here addressed by qualifier ion monitoring [29,30], and (2) correct quantification in the presence of significant ion suppression, which is best achieved by using properly matched stable isotope-labeled internal standards (SIL-IS) [31]. If properly applied, FIA-MS/MS provides high precision, short run times and remarkable cost savings due to elimination of time-consuming and possibly error-prone procedures of sample cleanup and pre-separation [27].…”

Section: Introductionmentioning

confidence: 99%

Determination of Creatinine in Human Urine with Flow Injection Tandem Mass Spectrometry

Niesser

Koletzko²,

Peißner³

2012

Ann Nutr Metab

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Background/Aims: Excretion of urinary compounds in spot urine is often estimated relative to creatinine. For the growing number of liquid chromatography-tandem mass spectrometry (LC-MS/MS) assays of urine-excreted molecules, a fast and accurate method for determination of creatinine is needed. Methods: A high-throughput flow injection tandem mass spectrometry method for exact quantitation of creatinine in urine has been developed and validated. Sample preparation used only two-step dilution for protein precipitation and matrix dilution. Flow injection analysis without chromatographic separation allowed for total run times of 1 min per sample. Creatinine concentrations were quantitated using stable isotope dilution tandem mass spectrometry. Selectivity and coelution-free quantitation were assured by qualifier ion monitoring. Results: Method validation revealed excellent injection repeatability of 1.0% coefficient of variation (CV), intraday precision of 1.2% CV and interday precision of 2.4% CV. Accuracy determined from standard addition experiments was 106.1 ± 3.8%. The linear calibration range was adapted to physiological creatinine concentrations. Comparison of quantitation results with a routinely used method (Jaffé colorimetric assay) proved high agreement (R² = 0.9102). Conclusions: The new method is a valuable addition to the toolbox of LC-MS/MS laboratories where excretion of urinary compounds is studied. The ‘dilute and shoot’ approach to isotope dilution tandem mass spectrometry makes the new method highly accurate as well as cost- and time-efficient.

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Fast screening of lovastatin in red yeast rice products by flow injection tandem mass spectrometry

Cited by 27 publications

References 15 publications

A Review of Current Trends and Advances in Analytical Methods for Determination of Statins: Chromatography and Capillary Electrophoresis

A Review of Current Trends and Advances in Analytical Methods for Determination of Statins: Chromatography and Capillary Electrophoresis

NMR evaluation of total statin content and HMG-CoA reductase inhibition in red yeast rice (Monascus spp.) food supplements

Determination of Creatinine in Human Urine with Flow Injection Tandem Mass Spectrometry

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