Quantification of natural products in herbal supplements: A combined NMR approach applied on goldenseal.

Abstract:

:Authentication of natural products is of major relevance in the context of manufactured drugs or herbal supplements since such active products generate a lucrative market. The analytical method to identify and quantify valuable natural products is critical for quality control and product assignment of herbal supplements. In this framework, we propose to apply a recently developed quantitative 2D NMR approach called Q QUIPU (Quick QUantItative Perfected and pUre shifted) in combination with 1D 1H NMR capable to access the concentration of three major alkaloids, berberine, β-hydrastine and canadine, in the root extract of goldenseal (Hydrastis canadensis), one of the 20 most popular herbal supplements used worldwide. We highlight the complementarity of 1D and 2D quantitative NMR to accurately assess the amount of alkaloids with different range of concentrations and stability within extracts. In particular, unstable natural products having non-overlapped signals like berberine could only be quantified by sensitive and fast 1D 1H, while overlapped signals of β-hydrastine and low intense ones of canadine could only be quantified with the recent 2D Q QUIPU HSQC. Results obtained from this combined approach have led to a good accuracy (<10%) as compared with coupled UHPLC-MS/UV techniques. This quantitative NMR approach paves the way to numerous applications where the accurate quantification of targeted compounds in complex mixtures is required, for instance in agricultural, food and pharmaceuticals products.

journal_name

J Pharm Biomed Anal

authors

Le PM,Milande C,Martineau E,Giraudeau P,Farjon J

doi

10.1016/j.jpba.2018.11.062

subject

Has Abstract

pub_date

2019-02-20 00:00:00

pages

155-161

eissn

0731-7085

issn

1873-264X

pii

S0731-7085(18)32371-9

journal_volume

165

pub_type

杂志文章
  • A comparative study of aurantio-obtusin metabolism in normal and liver-injured rats by ultra performance liquid chromatography quadrupole time-of-flight mass spectrometry.

    abstract::Aurantio-obtusin, an anthraquinone isolated from cassiae semen, possesses diverse pharmacological activities, including hypotensive, hypolipidemic and anti-inflammatory effects. However, our previous studies demonstrated that exposure to aurantio-obtusin induced hepatotoxicity, but the mechanisms of the toxic effects ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2021.113896

    authors: Xu L,Zhang Z,Hao F,Zhou W,Tang X,Gao Y

    更新日期:2021-01-13 00:00:00

  • Disorder of gut amino acids metabolism during CKD progression is related with gut microbiota dysbiosis and metagenome change.

    abstract::Chronic kidney disease (CKD) is a worldwide public health problem. Uremic retention solutes such as indoxyl sulfate (IS) and p-cresyl sulfate (PCS) are accumulated in CKD patients and are associated with the incidence of CKD progression. Amino acids are the major precursors of uremic retention solutes in gut. The dyna...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2017.11.040

    authors: Liu Y,Li J,Yu J,Wang Y,Lu J,Shang EX,Zhu Z,Guo J,Duan J

    更新日期:2018-02-05 00:00:00

  • Sensitive voltammetric determination of rutin at an in situ plated lead film electrode.

    abstract::A highly sensitive sensor for the determination of rutin by adsorptive stripping voltammetry was described. It consists of a lead film modified glassy carbon electrode (LF/GCE). In the proposed procedure rutin was accumulated by adsorption on the lead film electrode and then during the stripping step a lead film and t...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2008.11.022

    authors: Tyszczuk K

    更新日期:2009-02-20 00:00:00

  • Selective recognition of cis-trans-isomers of platinum drugs and the detection of triplex DNA based on fluorescence reversible model of quantum dots.

    abstract::The identification of spatial structures of drugs and the researches on their interaction mechanism with DNA are always attractive to the researchers. However, their realization is lack of simple and fast method. This paper reports the establishment of multiple-functional detection platform based on the "turn off-on" ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2016.11.033

    authors: Xu X,Gao F,Xiao X,Hu Y,Zhu C,Zhao D

    更新日期:2017-02-05 00:00:00

  • Spectrochemical identification of kanamycin resistance genes in artificial microbial communities using Clover-assay.

    abstract::Persistent abuse and overuse of antibiotics induces a widespread bloom of antibiotic resistance genes (ARGs) and the emergence of superbugs. A method designed to rapidly quantify ARGs in real-world scenarios is urgently needed. Here, we present an orthogonal test of heavy water and kanamycin exposure, namely, a "clove...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2020.113108

    authors: Jin N,Morais CLM,Martin FL,Zhang D

    更新日期:2020-03-20 00:00:00

  • Comprehensive phospholipid and sphingomyelin profiling of different brain regions in mouse model of anxiety disorder using online two-dimensional (HILIC/RP)-LC/MS method.

    abstract::A novel online system including two-dimensional liquid chromatography coupled to high-resolution mass spectrometry (2D-LC/MS) was developed and applied for comprehensive phospholipid (PL) and sphingomyelin (SM) profiling of dorsal hippocampus (DHPC), ventral (VHPC) and prefrontal cortex (PFC) brain regions in a mouse ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2017.10.043

    authors: Berkecz R,Tömösi F,Körmöczi T,Szegedi V,Horváth J,Janáky T

    更新日期:2018-02-05 00:00:00

  • Simultaneous quantification of cannabinoids tetrahydrocannabinol, cannabidiol and CB1 receptor antagonist in rat plasma: An application to characterize pharmacokinetics after passive cannabis smoke inhalation and co-administration of rimonabant.

    abstract::A highly sensitive and selective liquid chromatography-tandem mass spectrometry method for the determination of tetrahydrocannabinol (THC), cannabidiol, and rimonabant in rat plasma was developed. Analytes and the internal standard were extracted from plasma using a combination of protein precipitation followed by liq...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2018.07.004

    authors: Ravula A,Chandasana H,Setlow B,Febo M,Bruijnzeel AW,Derendorf H

    更新日期:2018-10-25 00:00:00

  • Determination of SNX-2112, a selective Hsp90 inhibitor, in plasma samples by high-performance liquid chromatography and its application to pharmacokinetics in rats.

    abstract::A sensitive and specific reversed-phase high-performance liquid chromatography method with ultraviolet detection has been developed and validated for the identification and quantification of SNX-2112 in rat plasma. Following sample preparation using liquid-liquid extraction, the analytes were separated by the mobile p...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2010.06.031

    authors: Zhai QQ,Gong GQ,Luo Y,Wang QD,Xia M,Xing GW,Li YC,Jiang JH,Liu Z,Liu QY,Wang YF

    更新日期:2010-12-01 00:00:00

  • Gas-phase structural characterization of neuropeptides Y Y1 receptor antagonists using mass spectrometry: Orbitrap vs triple quadrupole.

    abstract::Collision induced dissociation of triple quadrupole mass spectrometer (CID-QqQ) and high-energy collision dissociation (HCD) of Orbitrap were compared for four neuropeptides Y Y1 (NPY Y1) receptor antagonists and showed similar qualitative fragmentation and structural information. Orbitrap high resolution and high mas...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2018.01.013

    authors: Silva EMP,Varandas PAMM,Melo T,Barros C,Alencastre IS,Barreiros L,Domingues P,Lamghari M,Domingues MRM,Segundo MA

    更新日期:2018-03-20 00:00:00

  • Analysis of unconjugated morphine, codeine, normorphine and morphine as glucuronides in small volumes of plasma from children.

    abstract::A sensitive method for the analysis of unconjugated morphine, codeine, normorphine and total morphine after hydrolysis of glucuronide conjugates is described. The method was applicable to 50-microliters volumes of plasma. The analytes were converted to heptafluorobutyryl (HFB) derivatives before analysis by gas chroma...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(94)00121-h

    authors: Watson DG,Su Q,Midgley JM,Doyle E,Morton NS

    更新日期:1995-01-01 00:00:00

  • Separation and structural elucidation of a new tadalafil analogue diethylaminopretadalafil included as an adulterant in a dietary supplement.

    abstract::A new tadalafil analogue was detected and isolated from a dietary supplement, the structure was elucidated by means of nuclear magnetic resonance (NMR) and mass spectroscopy. The compound was determined to be diethylaminopretadalafil, which might be derived from a precursor in the synthesis of tadalafil. ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2014.01.043

    authors: Zhang G,Yu Y,Wu X,Li J

    更新日期:2014-06-01 00:00:00

  • Influence of hydrolysis procedures on the urinary concentrations of codeine and morphine in relation to doping analysis.

    abstract::A method is described for the GC-NPD determination of urinary codeine and morphine after derivatization with trifluoroacetic anhydride. The lower limit for accurate quantitative determination was 0.05 microgram ml-1. After the oral administration of Bisolvon Griblettes corresponding to 30 mg codeine phosphate to seven...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(93)80026-w

    authors: Delbeke FT,Debackere M

    更新日期:1993-04-01 00:00:00

  • Analysis of ACE-inhibitors by CE using alkylsulfonic additives.

    abstract::Capillary electrophoresis (CE) was applied to the determination of angiotensin-converting enzyme (ACE) inhibitors in pharmaceuticals (tablets). Since a free solution CE system failed to reach a complete separation of closely related compounds (lisinopril, ramipril, benazepril, quinapril), alkylsulfonic additives (sodi...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(00)00240-5

    authors: Gotti R,Andrisano V,Cavrini V,Bertucci C,Furlanetto S

    更新日期:2000-04-01 00:00:00

  • Non-destructive quantitative analysis of risperidone in film-coated tablets.

    abstract::A simple, non-destructive, methodology based on FT-Raman spectroscopy was developed for the quantitative analysis of risperidone in commercially available film-coated tablets. A simple linear regression model was constructed based on standard tablets, prepared using the same manufacturing process as the commercially a...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2008.01.049

    authors: Orkoula MG,Kontoyannis CG

    更新日期:2008-07-15 00:00:00

  • Analytical method transfer: improving interpretability with ratio-based statistical approaches.

    abstract::After assay validation in an originating laboratory, an analytical method needs to be transferred to one or several production laboratories, because measured outcomes among the laboratories must agree. To state agreement, the locations (e.g. means) must be equivalent and the production laboratory must be non-inferior ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2012.10.032

    authors: Frömke C,Hothorn LA,Sczesny F,Onken J,Schneider M

    更新日期:2013-02-23 00:00:00

  • Aspects of the stability of isoindoles derived from the reaction of o-phthalaldehyde-ethanethiol with primary amino compounds.

    abstract::The stability of a series of fluorescent isoindoles formed under analytical conditions following the reaction of o-phthalaldehyde (OPA) and ethanethiol (ET) with a series of primary amines is reported. Increasing the bulk and degree of substitution of the isoindole N-substituent resulted in substantial increases in is...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(86)80056-5

    authors: Stobaugh JF,Repta AJ,Sternson LA

    更新日期:1986-01-01 00:00:00

  • Secondary metabolites of Seseli rigidum: Chemical composition plus antioxidant, antimicrobial and cholinesterase inhibition activity.

    abstract::Extracts of different polarity obtained from various plant parts (root, leaf, flower and fruit) of Seseli rigidum were studied by different antioxidant assays: DPPH and ABTS radical scavenging activity, by total reducing power method as well as via total content of flavonoids and polyphenols. Essential oils of all pla...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2015.03.015

    authors: Stankov-Jovanović VP,Ilić MD,Mitić VD,Mihajilov-Krstev TM,Simonović SR,Nikolić Mandić SD,Tabet JC,Cole RB

    更新日期:2015-01-01 00:00:00

  • Sensitive quantitation of low level free polysaccharide in conjugate vaccines by size exclusion chromatography-reverse phase liquid chromatography with UV detection.

    abstract::The level of free polysaccharide is a critical quality attribute of polysaccharide-protein conjugate vaccines. The work presented describes a simple and sensitive method for the determination of low level free polysaccharides in multiple polysaccharide-protein conjugates. The method utilizes a reverse phase (RP) colum...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2019.113043

    authors: Schuchmann DC,Hou W,Creahan J,He Y,Jones MT

    更新日期:2020-02-20 00:00:00

  • Time domain NMR as a new process monitoring method for characterization of pharmaceutical hydrates.

    abstract::Hydrates are of great pharmaceutical relevance and even though they have been characterized thoroughly by various analytical techniques, there is barely literature available on molecular mobility of the hydrate water studied by NMR relaxation in the time domain. The aim of this work was to examine the possibility of d...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2017.01.017

    authors: Schumacher SU,Rothenhäusler B,Willmann A,Thun J,Moog R,Kuentz M

    更新日期:2017-04-15 00:00:00

  • Distribution and metabolism of gastrodin in rat brain.

    abstract::Gastrodin is the major and bioactive component in Tianma (Gastrodia elata Bl.) and has sedative, anticonvulsive and neuroprotective effects. Since little is known about its neuropharmacokinetics and brain metabolism, this study was undertaken to investigate the kinetic inter-relationship of gastrodin in rat plasma, ce...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2007.10.017

    authors: Wang Q,Chen G,Zeng S

    更新日期:2008-01-22 00:00:00

  • Thermospray liquid chromatography/mass spectrometry study of diastereomeric isoindole derivatives of amino acids and amino acid amides.

    abstract::A thermospray liquid chromatography/mass spectrometry (TSP-LC/MS) method is described for determination of the enantiomeric excess of alpha-amino acids and alpha-amino acid amides as their o-phthalaldehyde/N-acetyl-L-cysteine (OPA/NAC) derivatives. The source temperature is an important factor in optimizing the sensit...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(95)01580-9

    authors: van Leuken RG,Duchateau AL,Kwakkenbos GT

    更新日期:1995-11-01 00:00:00

  • Investigation of fatty acid esters to replace isopropyl myristate in the sterility test for ophthalmic ointments.

    abstract::Several pharmacopoeias recommend the membrane filtration method for the sterility test of ophthalmic ointments. Isopropyl myristate, a fatty acid ester that exhibits high toxicity mainly against Gram-negative microorganisms, is indicated as a solvent for ointments. In this study, six fatty acid esters (diethyl adipate...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2006.05.018

    authors: Cardoso VM,Solano AG,Prado MA,Nunan Ede A

    更新日期:2006-11-16 00:00:00

  • HPLC determination of sertraline in bulk drug, tablets and capsules using hydroxypropyl-beta-cyclodextrin as mobile phase additive.

    abstract::A sensitive and stereospecific high-performance liquid chromatography (HPLC) method for determination of sertraline in bulk drug, tablets and capsules was developed. Chromatography resolution of the sertraline enantiomeric forms and trans diastereoisomers was performed on Alltima C18 (250 mm x 4.6mm i.d., 5 microm) co...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.japna.2003.08.013

    authors: Chen D,Jiang S,Chen Y,Hu Y

    更新日期:2004-01-27 00:00:00

  • Simultaneous HPLC determination of ketoprofen and its degradation products in the presence of preservatives in pharmaceuticals.

    abstract::A novel and quick high-performance liquid chromatography (HPLC) method with UV spectrophotometric detection was developed and validated for the determination of five compounds in topical gel. The described method is suitable for simultaneous determination of active component ketoprofen, two preservatives methylparaben...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2004.07.018

    authors: Dvorák J,Hájková R,Matysová L,Nováková L,Koupparis MA,Solich P

    更新日期:2004-11-15 00:00:00

  • Reversed phase HPLC of Met58 oxidized rhIL-11: oxidation enhanced by plastic tubes.

    abstract::The hydrophobicity of human recombinant interleukin 11 (rhIL-11) with an oxidized Met58 residue is nearly identical to the hydrophobicity of native rhIL-11. Consequently, separation of these species using standard gradient elution or isocratic elution is very difficult. Using an optimized, shallow gradient RP-HPLC met...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(00)00419-2

    authors: Yokota H,Saito H,Masuoka K,Kaniwa H,Shibanuma T

    更新日期:2000-12-15 00:00:00

  • Development of a radioimmunoassay for RX77368 (pGlu-His-3,3-dimethyl proline amide)--a stable analogue of thyrotrophin releasing hormone (TRH).

    abstract::The recent interest in RX77368 for the treatment of Motor Neurone Disease (MND) has led to the requirement for an assay (RIA) capable of detecting the peptide at low levels in plasma. Several drug conjugates were prepared in which RX77368 was covalently linked to larger proteins, e.g. bovine serum albumin, keyhole lim...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(91)80230-7

    authors: Lynn AG,Bennett GW

    更新日期:1991-01-01 00:00:00

  • High-performance liquid chromatographic mapping of the oligosaccharides released from the humanised immunoglobulin, CAMPATH 1H.

    abstract::A sensitive and reproducible method for the routine mapping of oligosaccharides in a humanised immunoglobulin (IgG) is described. The method involves the enzymic release of intact glycans using the endoglycosidase glycopeptidase-F, and subsequent derivatisation with 1-phenyl-3-methyl-5-pyrazolone to facilitate analysi...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(95)01646-5

    authors: Lines AC

    更新日期:1996-03-01 00:00:00

  • An HPLC assay for the norditerpenoid alkaloid methyllycaconitine, a potent nicotinic acetylcholine receptor antagonist.

    abstract::The extremely potent and selective nicotinic acetylcholine receptor antagonist methyllycaconitine, MLA, and related norditerpene alkaloids are finding increasing use as neurochemical probes and as targets for structure-activity relationship studies. In this work, an assay procedure for MLA which utilises ion suppressi...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(95)01599-x

    authors: Coates PA,Blagbrough IS,Lewis T,Potter BV,Rowan MG

    更新日期:1995-11-01 00:00:00

  • Characterization of a new illicit phosphodiesterase-type-5 inhibitor identified in the softgel shell of a dietary supplement.

    abstract::A new sildenafil analog has been identified in the softgel shell of a dietary supplement. The compound was investigated by UV spectroscopy and high-resolution MS analysis, leading to the proposed structure 1-methyl-5-{5-[2-(4-methylpiperazin-1-yl)acetyl]-2-propoxyphenyl}-3-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]pyrimidi...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2018.08.031

    authors: Doi T,Takahashi K,Yamazaki M,Asada A,Takeda A,Kiyota K,Tagami T,Sawabe Y,Yamano T

    更新日期:2018-11-30 00:00:00

  • Analysis of phenolics in wine by high performance thin-layer chromatography with gradient elution and high resolution plate imaging.

    abstract::Health benefits of wine, especially with red wine, have been linked to the presence of a wide range of phenolic antioxidants. Thus, the aim of this study was to develop a simple, high performance thin layer chromatographic (HPTLC) method combined with high resolution digital plate images to visually compare multiple w...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2014.08.031

    authors: Agatonovic-Kustrin S,Hettiarachchi CG,Morton DW,Razic S

    更新日期:2015-01-01 00:00:00