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Analysis of lignans from Phyllanthus niruri L. in plasma using a simple HPLC method with fluorescence detection and its application in a pharmacokinetic study

Murugaiyah V, Chan KL

J Chromatogr B Analyt Technol Biomed Life Sci, 2007 Jun 1;852(1-2):138-44.
PMID: 17261384

A simple analytical method using HPLC with fluorescence detection was developed for the simultaneous determination of four lignans, phyllanthin (1), hypophyllanthin (2), phyltetralin (3) and niranthin (4) from Phyllanthus niruri L. in plasma. The method recorded limits of detection for 1, 2, 3 and 4 as 1.22, 6.02, 0.61 and 1.22 ng/ml, respectively, at a signal-to-noise ratio of 5:1 whereas their limits of quantification were 4.88, 24.41, 4.88 and 9.76 ng/ml, respectively, at a signal-to-noise ratio of 12:1. These values were comparable to those of other sensitive methods such as gas chromatography-mass spectrometry (GC-MS), high-performance liquid chromatography-MS (HPLC-MS) and HPLC-electrochemical detection (HPLC-ECD) for the analysis of plasma lignans. A further advantage over known methods was its simple protocol for sample preparation. The within-day and between-day accuracies for the analysis of the four lignans were between 87.69 and 110.07% with precision values below 10.51%. Their mean recoveries from extraction were between 91.39 and 114.67%. The method was successfully applied in the pharmacokinetic study of lignans in rats. Following intravenous administration, the lignans were eliminated slowly from the body with a mean clearance of 0.04, 0.01, 0.03 and 0.02 l/kg h and a mean half-life of 3.56, 3.87, 3.35 and 4.40 h for 1, 2, 3 and 4, respectively. Their peak plasma concentration upon oral administration was 0.18, 0.56, 0.12 and 0.62 microg/ml, respectively, after 1h. However, their absorption was incomplete with a calculated absolute oral bioavailability of 0.62, 1.52, 4.01 and 2.66% for 1, 2, 3 and 4, respectively.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
Simple, rapid and sensitive assay method for simultaneous quantification of urinary nicotine and cotinine using gas chromatography-mass spectrometry

Man CN, Gam LH, Ismail S, Lajis R, Awang R

J Chromatogr B Analyt Technol Biomed Life Sci, 2006 Dec 5;844(2):322-7.
PMID: 16908224

Nicotine is a major addictive compound in cigarette. Its smoke is rapidly and extensively metabolized to several metabolites in human. Cotinine as a major metabolite of nicotine is commonly used as a biomarker to determine active and passive smokers. Cotinine has a longer half-life ( approximately 20 h) compared to nicotine ( approximately 2h). A simple, sensitive, rapid and high throughput GC-MS method was developed for simultaneous quantification of urinary nicotine and cotinine in passive and active smokers. In the sample preparation method, the analytes and internal standard were first basified and followed by liquid-liquid extraction. Upon completion, anhydrous sodium sulphate was added to the solvent mixture to trap moistures. The clear extract obtained was directly injected into GC-MS, operating under selective ion monitoring (SIM) mode. Calibration curves in the range of 0.5-5000 ng/mL of the analytes in urine matrix were established with linear correlation coefficients (r(2)) greater than 0.997. The limit of detection for both nicotine and cotinine were 0.20 ng/mL. The mean recoveries for nicotine and cotinine were 93.0 and 100.4%, respectively. The within- and between-assay accuracies were between 2.1 and 7.9% for nicotine and between 0.7 and 11.1% for cotinine. Within- and between-assay precisions of 3.3-9.5% for nicotine and 3.4-9.8% for cotinine were also achieved. The method can be used in routine assessment and monitoring of active smoking and exposure to environmental tobacco smoke. The applicability of the assay was demonstrated in a small-scale comparison study between smokers and non-smokers.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry/methods*
Liquid chromatographic method for the determination of plasma itraconazole and its hydroxy metabolite in pharmacokinetic/bioavailability studies

Wong JW, Nisar UR, Yuen KH

J Chromatogr B Analyt Technol Biomed Life Sci, 2003 Dec 25;798(2):355-60.
PMID: 14643517

A sensitive and selective high-performance liquid chromatographic method was developed for the determination of itraconazole and its active metabolite, hydroxyitraconazole, in human plasma. Prior to analysis, both compounds together with the internal standard were extracted from alkalinized plasma samples using a 3:2 (v/v) mixture of 2,2,4-trimethylpentane and dichloromethane. The mobile phase comprised 0.02 M potassium dihydrogen phosphate-acetonitrile (1:1, v/v) adjusted to pH 3.0. Analysis was run at flow-rate of 0.9 ml/min with excitation and emission wavelengths set at 260 and 365 nm, respectively. Itraconazole was found to adsorb on glass or plastic tubes, but could be circumvented by prior treating the tubes using 10% dichlorodimethylsilane in toluene. Moreover, rinsing the injector port with acetonitrile helped to overcome any carry-over effect. This problem was not encountered with hydroxyitraconazole. The method was sensitive with limit of quantification of 3 ng/ml for itraconazole and 6 ng/ml for hydroxyitraconazole. The calibration curve was linear over a concentration range of 2.8-720 ng/ml for itraconazole and 5.6-720 ng/ml for the hydroxy metabolite. Mean recovery value of the extraction procedure for both compounds was about 85%, while the within-day and between-day coefficient of variation and percent error values of the assay method were all less than 15%. Hence, the method is suitable for use in pharmacokinetic and bioavailability studies of itraconazole.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
Purification of bacteriophage M13 by anion exchange chromatography

Monjezi R, Tey BT, Sieo CC, Tan WS

J Chromatogr B Analyt Technol Biomed Life Sci, 2010 Jul 1;878(21):1855-9.
PMID: 20538529 DOI: 10.1016/j.jchromb.2010.05.028

M13 is a non-lytic filamentous bacteriophage (phage). It has been used widely in phage display technology for displaying foreign peptides, and also for studying macromolecule structures and interactions. Traditionally, this phage has been purified by cesium chloride (CsCl) density gradient ultracentrifugation which is highly laborious and time consuming. In the present study, a simple, rapid and efficient method for the purification of M13 based on anion exchange chromatography was established. A pre-packed SepFast Super Q column connected to a fast protein liquid chromatography (FPLC) system was employed to capture released phages in clarified Escherichia coli fermented broth. An average yield of 74% was obtained from a packed bed mode elution using citrate buffer (pH 4), containing 1.5 M NaCl at 1 ml/min flow rate. The purification process was shortened substantially to less than 2 h from 18 h in the conventional ultracentrifugation method. SDS-PAGE revealed that the purity of particles was comparable to that of CsCl gradient density ultracentrifugation method. Plaque forming assay showed that the purified phages were still infectious.

Matched MeSH terms: Chromatography, Ion Exchange/methods*
Determination of hair nicotine by gas chromatography-mass spectrometry

Man CN, Ismail S, Harn GL, Lajis R, Awang R

J Chromatogr B Analyt Technol Biomed Life Sci, 2009 Jan 15;877(3):339-42.
PMID: 19109080 DOI: 10.1016/j.jchromb.2008.12.014

Hair nicotine is a known biomarker for monitoring long-term environmental tobacco smoke (ETS) exposure and smoking status. In general, hair nicotine assay involves alkaline digestion, extraction and instrumental analysis. The gas chromatography-mass spectrometry (GC-MS) assay currently developed has shown to be of high throughput with average approximately 100 hair samples being extracted and analyzed per day. This was achieved through simplified extraction procedure and shortened GC analysis time. The extraction was improved by using small volume (0.4 mL) of organic solvent that does not require further evaporation and salting steps prior to GC-MS analysis. Furthermore, the amount of hair utilized in the extraction was very little (5 mg) while the sensitivity and selectivity of the assay is equal, if not better than other established methods. The linearity of the assay (r(2)>0.995), limit of quantitation (0.04 ng/mg hair), within- and between-assays accuracies and precisions (<11.4%) and mean recovery (92.6%) were within the acceptable range.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry*
Hollow fiber liquid-phase microextraction combined with high performance liquid chromatography for the determination of trace mitiglinide in biological fluids

Hadi H, Makahleh A, Saad B

J Chromatogr B Analyt Technol Biomed Life Sci, 2012 May 1;895-896:131-6.
PMID: 22503735 DOI: 10.1016/j.jchromb.2012.03.031

A hollow fiber liquid phase microextraction (HF-LPME) in conjunction with reversed phase HPLC-UV method was developed for the extraction and determination of trace amounts of the antidiabetic drug, mitiglinide (MIT) in biological fluids. The drug was extracted from 10 mL aqueous sample (donor phase (DP)) into an organic phase impregnated in the pores of hollow fiber, followed by the back extraction into a second aqueous solution (acceptor phase (AP)) located in the lumen of the hollow fiber. Parameters influencing the extraction efficiency including the kind of organic solvent, composition of DP and AP, extraction time, stirring rate and salt addition were investigated and optimized. Under the optimized extraction conditions, high enrichment factors (210-fold), good linearity (5-1000 ng mL(-1)) and detection limit lower than 1.38 ng mL(-1) were achieved. Recoveries of spiked samples were in the range (88.3-96.3%) and (92.0-99.3%) for urine and plasma samples, respectively. The percent relative standard deviation (n=9) for the extraction and determination of three concentration levels (100, 400 and 800 ng mL(-1)) of MIT were less than 10.6% and 13.6% for urine and plasma samples, respectively. The developed method is simple, sensitive and has been successfully applied to the analysis of MIT in biological fluids.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
Chiral liquid chromatography-mass spectrometry (LC-MS/MS) method development for the detection of salbutamol in urine samples

Chan SH, Lee W, Asmawi MZ, Tan SC

J Chromatogr B Analyt Technol Biomed Life Sci, 2016 Jul 01;1025:83-91.
PMID: 27232053 DOI: 10.1016/j.jchromb.2016.05.015

A sequential solid-phase extraction (SPE) method was developed and validated using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) for the detection and quantification of salbutamol enantiomers in porcine urine. Porcine urine samples were hydrolysed with β-glucuronidase/arylsulfatase from Helix pomatia and then subjected to a double solid-phase extraction (SPE) first using the Abs-Elut Nexus SPE and then followed by the Bond Elut Phenylboronic Acid (PBA) SPE. The salbutamol enantiomers were separated using the Astec CHIROBIOTIC™ T HPLC column (3.0mm×100mm; 5μm) maintained at 15°C with a 15min isocratic run at a flow rate of 0.4mL/min. The mobile phase constituted of 5mM ammonium formate in methanol. Salbutamol and salbutamol-tert-butyl-d9 (internal standard, IS) was monitored and quantified with the multiple reaction monitoring (MRM) mode. The method showed good linearity for the range of 0.1-10ng/mL with limit of quantification at 0.3ng/mL. Analysis of the QC samples showed intra- and inter-assay precisions to be less than 5.04%, and recovery ranging from 83.82 to 102.33%.

Matched MeSH terms: Chromatography, Liquid/methods*
Method development and validation of a high-performance liquid chromatographic method for tramadol in human plasma using liquid-liquid extraction

Gan SH, Ismail R, Wan Adnan WA, Wan Z

J Chromatogr B Analyt Technol Biomed Life Sci, 2002 May 25;772(1):123-9.
PMID: 12016023

An HPLC system using a simple liquid-liquid extraction and HPLC with UV detection has been validated to determine tramadol concentration in human plasma. The method developed was selective and linear for concentrations ranging from 10 to 2000 ng/ml with average recovery of 98.63%. The limit of quantitation (LOQ) was 10 ng/ml and the percentage recovery of the internal standard phenacetin was 76.51%. The intra-day accuracy ranged from 87.55 to 105.99% and the inter-day accuracy, 93.44 to 98.43% for tramadol. Good precision (5.32 and 6.67% for intra- and inter-day, respectively) was obtained at LOQ. The method has been applied to determine tramadol concentrations in human plasma samples for a pharmacokinetic study.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
Fulltext Stability of glycated haemoglobin (HbA1c) measurements from whole blood samples kept at -196°C for seven to eight years in The Malaysian Cohort study

Abdullah N, Goh YX, Othman R, Ismail N, Jalal N, Wan Sallam WAF, et al.

J Clin Lab Anal, 2023 Apr;37(8):e24898.
PMID: 37243371 DOI: 10.1002/jcla.24898

OBJECTIVE: Glycated haemoglobin (HbA1c) is a standard indication for screening type 2 diabetes that also has been widely used in large-scale epidemiological studies. However, its long-term quality (in terms of reproducibility) stored in liquid nitrogen is still unknown. This study is aimed to evaluate the stability and reproducibility of HbA1c measurements from frozen whole blood samples kept at -196°C for more than 7 years.
METHODS: A total of 401 whole blood samples with a fresh HbA1c measurement were randomly selected from The Malaysian Cohort's (TMC) biobank. The HbA1c measurements of fresh and frozen (stored for 7-8 years) samples were assayed using different high-performance liquid chromatography (HPLC) systems. The HbA1c values of the fresh samples were then calculated and corrected according to the later system. The reproducibility of HbA1c measurements between calculated-fresh and frozen samples was assessed using a Passing-Bablok linear regression model. The Bland-Altman plot was then used to evaluate the concordance of HbA1c values.
RESULTS: The different HPLC systems highly correlated (r = 0.99) and agreed (ICC = 0.96) with each other. Furthermore, the HbA1c measurements for frozen samples strongly correlate with the corrected HbA1c values of the fresh samples (r = 0.875) with a mean difference of -0.02 (SD: -0.38 to 0.38). Although the mean difference is small, discrepancies were observed within the diabetic and non-diabetic samples.
CONCLUSION: These data demonstrate that the HbA1c measurements between fresh and frozen samples are highly correlated and reproducible.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods
Fulltext Identification of hemoglobin AC heterozygote status in a Malay family: a decision between hemoglobin electrophoresis and high performance liquid chromotography

Rosline H, Roshan TM, Ahmed SA, Ilunihayati I

Southeast Asian J Trop Med Public Health, 2007 May;38(3):543-5.
PMID: 17877232

Thalassemia is a common public health problem among Malays. Hemoglobin C (Hb C) is a hemoglobin beta variant resulting from a single base mutation at the 6th position of the beta-globin gene leading to the substitution of glycine for glutamic acid. Hb C is commonly detected in West Africans and in African American but has not been reported in Malaysia. It can be falsely diagnosed as HbE trait in the Malaysian Thalassemia Screening Program which utilizes cellulose acetate hemoglobin electrophoresis. This is the first reported case of Hb AC heterozygote status in a Malay family, with unusual splenomegaly in one of the family members.

Matched MeSH terms: Chromatography, High Pressure Liquid*
Fulltext Does sildenafil citrate affect the pharmacokinetics of metformin in rats? Screening of mechanism through analytical and molecular docking approach

Dewani AP, Rab SO, Tripathi P, Shrivastava S, Tripathi R, Tripathi AS, et al.

Indian J Pharmacol, 2024 May 01;56(3):178-185.
PMID: 39078181 DOI: 10.4103/ijp.ijp_562_23

OBJECTIVE: In the present study, the effect of sildenafil on the pharmacokinetics of metformin was studied in experimental rats, and we also postulated the molecular mechanism by performing molecular docking studies.
MATERIALS AND METHODS: Analysis of metformin and sildenafil (SIL) from rat plasma was done by high performance liquid chromatography. Optimum chromatographic separation and quantification of MET, SIL and Cetirizine was achieved on Phenomenex EVO C18 column with triethyl amine (0.3%): Methanol: Acetonitrile (70:05:25 v/v) as mobile phase maintaining flow rate of 1 ml/min, the detector was tuned at 224 nm. The extraction of MET and sildenafil from rat plasma was achieved by solid-phase extraction using Strata-X cartridges. The method was validated as per the ICH guidelines. For docking studies, the crystal structure of organic cation transporter 1 (OCT1) protein and multidrug and toxin extrusion (MATE) protein (5XJJ) were downloaded from the PubChem database. The docking study was performed by PyRx virtual screening software, and the results were analyzed by BIOVIA Discovery Studio.
RESULTS: The validation of HPLC method was done, intraday and interday precision study of HPLC method demonstrated %RSD values less than 5%, the extraction recovery for MET and SIL were near to 80 % for low, medium and high QC samples. The plasma stability of MET and SIL showed % RSD values <10% for low, medium, and high QC samples. A sensitivity study for MET and SIL in rat plasma suggested a lower limit of quantification values of 8 and 10 ng/mL, respectively. The pharmacokinetic parameters were recorded, Cmax of experimental and control rats was 611.2 and 913.2 ng/mL; t1/2 1.66 and 1.98, AUC (0-t) 1637.5 and 2727.24, AUC (0-∞) 1832.38 and 2995.24 for MET. The results suggested that the Cmax of MET in experimental rats (MET + SIL) was 33.07% lower than the control (MET only) and also the t1/2 was 0.32 h shorter. Docking analysis suggested a higher binding affinity of sildenafil with MATE protein (5XJJ) compared to OCT1, suggesting possible involvement of MATE family proteins for pharmacokinetic alterations of MET.
CONCLUSIONS: The HPLC and solid-phase extraction method were developed and applied successfully for the pharmacokinetics of MET and SIL. Intake of SIL altered the pharmacokinetics of MET in rats. Molecular docking studies suggested the involvement of MATE family proteins for alterations of MET pharmacokinetics.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods
Fulltext Identification and concentration of some flavonoid components in Malaysian young ginger (Zingiber officinale Roscoe) varieties by a high performance liquid chromatography method

Ghasemzadeh A, Jaafar HZ, Rahmat A

Molecules, 2010 Sep 03;15(9):6231-43.
PMID: 20877219 DOI: 10.3390/molecules15096231

Flavonoids make up one of the most pervasive groups of plant phenolics. Due to their importance in plants and human health, it would be useful to have a better understanding of flavonoid concentration and biological activities that could indicate their potentials as therapeutic agents, and also for predicting and controlling the quality of medicinal herbs. Ginger (Zingiber officinale Roscoe) is a famous and widely used herb, especially in Asia, that contains several interesting bioactive constituents and possesses health promoting properties. In this study, total flavonoids and some flavonoid components including quercetin, rutin, catechin, epicatechin, kaempferol and naringenin were extracted from the leaves and rhizomes of two varieties of Zingiber officinale (Halia Bentong and Halia Bara) at three different growth points (8, 12 and 16 weeks after planting), and analyzed by a high performance liquid chromatography (HPLC) method in order to determine the potential of the subterranean part of the young ginger. The results showed that Halia Bara had a higher content of flavonoids in the leaves and rhizomes as compared to Halia Bentong. In both varieties, the concentration of flavonoids in the leaves decreased (Halia Bentong, 42.3%; Halia Bara 36.7%), and in the rhizomes it increased (Halia Bentong 59.6%; Halia Bara 60.1%) as the growth period increased. Quercetin was abundant in both varieties. The antioxidant activity determined by the 1,1-diphenyl-2-picryl-hydrazyl (DPPH) assay showed high activities (65.7%) in the leaves of Halia Bara at 8 weeks after planting. Results suggested a good flavonoid content and antioxidant activity potential in ginger leaves at 8 weeks after planting. The leaves of these ginger varieties could be useful for both food flavourings and in traditional medicine.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods
Assessment of antioxidant activity in Victorian marine algal extracts using high performance thin-layer chromatography and multivariate analysis

Agatonovic-Kustrin S, Morton DW, Ristivojević P

J Chromatogr A, 2016 Oct 14;1468:228-235.
PMID: 27670751 DOI: 10.1016/j.chroma.2016.09.041

The aim of this study was to develop and validate a rapid and simple high performance thin layer chromatographic (HPTLC) method to screen for antioxidant activity in algal samples. 16 algal species were collected from local Victorian beaches. Fucoxanthin, one of the most abundant marine carotenoids was quantified directly from the HPTLC plates before derivatization, while derivatization either with 2,2-diphenyl-1-picrylhydrazyl (DPPH) or ferric chloride (FeCl3) was used to analyze antioxidants in marine algae, based on their ability to scavenge non biological stable free radical (DPPH) or to chelate iron ions. Principal component analysis of obtained HPTLC fingerprints has classified algae species into 5 groups according to their chemical/antioxidant profiles. The investigated brown algae samples were found to be rich in non-and moderate-polar compounds and phenolic compounds with antioxidant activity. Most of the phenolic iron chelators also have shown free radical scavenging activity. Strong positive and significant correlations between total phenolic content and DPPH radical scavenging activity showed that, phenolic compounds, including flavonoids are the main contributors of antioxidant activity in these species. The results suggest that certain brown algae possess significantly higher antioxidant potential when compared to red or green algae and could be considered for future applications in medicine, dietary supplements, cosmetics or food industries. Cystophora monilifera extract was found to have the highest antioxidant concentration, followed by Zonaria angustata, Cystophora pectinate, Codium fragile, and Cystophora pectinata. Fucoxanthin was found mainly in the brown algae species. The proposed methods provide an edge in terms of screening for antioxidants and quantification of antioxidant constituents in complex mixtures. The current application also demonstrates flexibility and versatility of a standard HPTLC system in the drug discovery. Proposed methods could be used for the bioassay-guided isolation of unknown natural antioxidants and subsequent identification if combined with spectroscopic identification.

Matched MeSH terms: Chromatography, Thin Layer/methods
Bioassay-guided detection, identification and assessment of antibacterial and anti-inflammatory compounds from olive tree flower extracts by high-performance thin-layer chromatography linked to spectroscopy

Agatonovic-Kustrin S, Wong S, Dolzhenko AV, Gegechkori V, Morton DW

J Pharm Biomed Anal, 2024 Feb 15;239:115912.
PMID: 38128161 DOI: 10.1016/j.jpba.2023.115912

Olive trees are one of the most widely cultivated fruit trees in the world. The chemical compositions and biological activities of olive tree fruit and leaves have been extensively researched for their nutritional and health-promoting properties. In contrast, limited data have been reported on olive flowers. The present study aimed to analyse bioactive compounds in olive flower extracts and the effect of fermentation-assisted extraction on phenolic content and antioxidant activity. High-performance thin-layer chromatography (HPTLC) hyphenated with the bioassay-guided detection and spectroscopic identification of bioactive compounds was used for the analysis. Enzymatic and bacterial in situ bioassays were used to detect COX-1 enzyme inhibition and antibacterial activity. Multiple zones of antibacterial activity and one zone of COX-1 inhibition were detected in both, non-fermented and fermented, extracts. A newly developed HPTLC-based experimental protocol was used to measure the high-maximal inhibitory concentrations (IC50) for the assessment of the relative potency of the extracts in inhibiting COX-1 enzyme and antibacterial activity. Strong antibacterial activities detected in zones 4 and 7 were significantly higher in comparison to ampicillin, as confirmed by low IC50 values (IC50 = 57-58 µg in zone 4 and IC50 = 157-167 µg in zone 7) compared to the ampicillin IC50 value (IC50 = 495 µg). The COX-1 inhibition by the extract (IC50 = 76-98 µg) was also strong compared to that of salicylic acid (IC50 = 557 µg). By comparing the locations of the bands to coeluted standards, compounds from detected bioactive bands were tentatively identified. The eluates from bioactive HPTLC zones were further analysed by FTIR NMR, and LC-MS spectroscopy. Multiple zones of antibacterial activity were associated with the presence of triterpenoid acids, while COX-1 inhibition was related to the presence of long-chain fatty acids.

Matched MeSH terms: Chromatography, Thin Layer/methods
Gas Chromatography-Mass Spectrometry (GC-MS) Analysis of Scaphium Affine Seed Extract and Assessment of Its Anti-hemorrhoidal Efficacy

Abbas SA, Khan A, Fatima M, Kalusalingam A, Kanakal MM, Inamdar SK, et al.

Antiinflamm Antiallergy Agents Med Chem, 2024;23(2):118-128.
PMID: 38357954 DOI: 10.2174/0118715230285370240131111539

BACKGROUND: Seeds of plant Scaphium affine are traditionally used by the healers of "India" for the treatment of piles.
OBJECTIVES: The primary objective of the study was to assess the anti-hemorrhoidal potential of the ethanolic seed extract of Scaphium affine.
METHODS: After the soxhlet extraction method, the seed extract from Scaphium affine was first submitted to phytochemical standardization and then GC-MS analysis. Rats were given Croton oil and Jatropha oil to develop hemorrhoids, and Scaphium affine seed extract (ESA) was administered orally for 5 days and 3 days, respectively, at doses of 1000 and 500 mg/kg. The Rectoanal coefficient (RAC) was calculated as an inflammatory marker. The hemorrhoidal tissues were also subjected to cytokine profiling, biochemical estimation and histopathology.
RESULTS: ESA demonstrated the presence of flavonoids, saponins, phytosterols, phenols, and tannins. GCMS analysis elucidated the presence of hexadecanoic acid 2 hydroxy -1,3 propane diyl ester,9 Octadecanoic acid ethyl ester, Cyclohexane 1,4 di methyl cis, Farnesol isomer,1, E-11, Z-13 octa decatriene, Stigmasterol, N-(5 ethyl -1,3,4-thiadiazol-yl) benzamide, N, N Dinitro 1,3,5,7 tetraza bicyclo 93,3,1) as major phytoconstituents. The results depicted more potent anti-hemorrhoidal activity of ESA at 1000 mg/kg, p.o., which was evident through a decrease in RAC. A significant decline in the levels of IL-1β, IL-6, and TNF-α expression was observed, along with the restoration of altered antioxidants and enzymes. Histopathological analysis confirmed the tissue recovery as it revealed minimal inflammation and decreased dilated blood vessels in treated animals.
CONCLUSION: Based on the results it can be concluded that seeds of Scaphium affine showed significant anti-hemorrhoid agents which may be attributed to their anti-inflammatory and anti-oxidant potential due to the presence of certain phytoconstituents in it. The study also supports the traditional use of seeds of Scaphium affine for the first time in the treatment of hemorrhoids.

Matched MeSH terms: Gas Chromatography-Mass Spectrometry*
Use of tryptic peptide MALDI mass spectrometry imaging to identify the spatial proteomic landscape of colorectal cancer liver metastases

Li CMY, Briggs MT, Lee YR, Tin T, Young C, Pierides J, et al.

Clin Exp Med, 2024 Mar 16;24(1):53.
PMID: 38492056 DOI: 10.1007/s10238-024-01311-5

Colorectal cancer (CRC) is the second leading cause of cancer-related deaths worldwide. CRC liver metastases (CRLM) are often resistant to conventional treatments, with high rates of recurrence. Therefore, it is crucial to identify biomarkers for CRLM patients that predict cancer progression. This study utilised matrix-assisted laser desorption/ionisation mass spectrometry imaging (MALDI-MSI) in combination with liquid chromatography-tandem mass spectrometry (LC-MS/MS) to spatially map the CRLM tumour proteome. CRLM tissue microarrays (TMAs) of 84 patients were analysed using tryptic peptide MALDI-MSI to spatially monitor peptide abundances across CRLM tissues. Abundance of peptides was compared between tumour vs stroma, male vs female and across three groups of patients based on overall survival (0-3 years, 4-6 years, and 7+ years). Peptides were then characterised and matched using LC-MS/MS. A total of 471 potential peptides were identified by MALDI-MSI. Our results show that two unidentified m/z values (1589.876 and 1092.727) had significantly higher intensities in tumours compared to stroma. Ten m/z values were identified to have correlation with biological sex. Survival analysis identified three peptides (Histone H4, Haemoglobin subunit alpha, and Inosine-5'-monophosphate dehydrogenase 2) and two unidentified m/z values (1305.840 and 1661.060) that were significantly higher in patients with shorter survival (0-3 years relative to 4-6 years and 7+ years). This is the first study using MALDI-MSI, combined with LC-MS/MS, on a large cohort of CRLM patients to identify the spatial proteome in this malignancy. Further, we identify several protein candidates that may be suitable for drug targeting or for future prognostic biomarker development.

Matched MeSH terms: Chromatography, Liquid/methods
Purification of long helical capsid of newcastle disease virus from Escherichia coli using anion exchange chromatography

Yap CF, Tan WS, Sieo CC, Tey BT

Biotechnol Prog, 2013 Mar-Apr;29(2):564-7.
PMID: 23364925 DOI: 10.1002/btpr.1697

NP(Δc375) is a truncated version of the nucleocapsid protein of Newcastle disease virus (NDV) which self-assembles into a long helical structure. A packed bed anion exchange chromatography (PB-AEC), SepFastTM Supor Q pre-packed column, was used to purify NP(Δc375) from clarified feedstock. This PB-AEC column adsorbed 76.2% of NP(Δc375) from the clarified feedstock. About 67.5% of the adsorbed NP(Δc375) was successfully eluted from the column by applying 50 mM Tris-HCl elution buffer supplemented with 0.5 M NaCl at pH 7. Thus, a recovery yield of 51.4% with a purity of 76.7% which corresponds to a purification factor of 6.5 was achieved in this PB-AEC operation. Electron microscopic analysis revealed that the helical structure of the NP(Δc375) purified by SepFast(TM) Supor Q pre-packed column was as long as 490 nm and 22-24 nm in diameter. The antigenicity of the purified NP(Δc375) was confirmed by enzyme-linked immunosorbent assay.

Matched MeSH terms: Chromatography, Ion Exchange/instrumentation; Chromatography, Ion Exchange/methods*
Structure-activity relationship of polyisoprenyl benzophenones from Garcinia pyrifera on the tubulin/microtubule system

Roux D, Hadi HA, Thoret S, Guénard D, Thoison O, Païs M, et al.

J Nat Prod, 2000 Aug;63(8):1070-6.
PMID: 10978200

Microtubule disassembly inhibitory properties have been established for the known polyisoprenylated benzophenones xanthochymol (1a) and guttiferone E (1b). The compounds were isolated from the fruits of Garcinia pyrifera collected in Malaysia. A structure-activity relationship study, including natural and semisynthetic derivatives, delineated some structural features necessary for the interaction with tubulin within this compound class.

Matched MeSH terms: Chromatography, Gel; Chromatography, High Pressure Liquid; Gas Chromatography-Mass Spectrometry
α-glucosidase inhibitors isolated from Mimosa pudica L

Tasnuva ST, Qamar UA, Ghafoor K, Sahena F, Jahurul MHA, Rukshana AH, et al.

Nat Prod Res, 2019 May;33(10):1495-1499.
PMID: 29281898 DOI: 10.1080/14786419.2017.1419224

The aim of the study was to isolate digestive enzymes inhibitors from Mimosa pudica through a bioassay-guided fractionation approach. Repeated silica gel and sephadex LH 20 column chromatographies of bioactive fractions afforded stigmasterol, quercetin and avicularin as digestive enzymes inhibitors whose IC50 values as compared to acarbose (351.02 ± 1.46 μg mL-1) were found to be as 91.08 ± 1.54, 75.16 ± 0.92 and 481.7 ± 0.703 μg mL-1, respectively. In conclusion, M. pudica could be a good and safe source of digestive enzymes inhibitors for the management of diabetes in future.

Matched MeSH terms: Chromatography, Liquid/instrumentation; Chromatography, Liquid/methods
Method development and validation for the simultaneous determination of imatinib mesylate and N-desmethyl imatinib using rapid resolution high performance liquid chromatography coupled with UV-detection

Tan KL, Ankathil R, Gan SH

J Chromatogr B Analyt Technol Biomed Life Sci, 2011 Nov 15;879(30):3583-91.
PMID: 22000961 DOI: 10.1016/j.jchromb.2011.09.048

We developed a simple and sensitive method for the simultaneous detection of imatinib mesylate (IM) and its active metabolite, N-desmethyl imatinib (M1), in human serum samples. Separation was successfully achieved using an Agilent(®) ZORBAX Eclipse plus C(18) reversed phase column (50 mm × 2.1 mm, i.d.; 1.8 μm) under isocratic mobile phase conditions consisting of acetonitrile: 0.02 M potassium dihydrogen phosphate with 0.2% triethylamine at pH 3 (25:75, v/v) and ultra-violet detection was achieved at 235 nm. Extraction of the target compounds was completed using 100% cold acetonitrile. Good linearities (r(2)>0.99) for both IM and M1 were achieved for the concentration ranges of 50-1800 ng/mL and 50-360 ng/mL, respectively. The detection limits were 20 ng/mL and 10 ng/mL for M1 and IM, respectively. The intra- and inter-day precisions were less than 1% with percent recoveries of more than 90%. The method was successfully applied to calculate the pharmacokinetic parameters of chronic myeloid leukemia patients receiving imatinib. The method is suitable to be routinely applied for determination of IM and M1 in serum.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*; Chromatography, Reverse-Phase

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