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In situ derivatization hollow fibre liquid-phase microextraction for the determination of biogenic amines in food samples

Saaid M, Saad B, Ali AS, Saleh MI, Basheer C, Lee HK

J Chromatogr A, 2009 Jul 3;1216(27):5165-70.
PMID: 19481215 DOI: 10.1016/j.chroma.2009.04.091

Hollow fibre liquid-phase microextraction with in situ derivatization using dansyl chloride has been successfully developed for the high-performance liquid chromatography-ultraviolet (HPLC-UV) determination of the biogenic amines (tryptamine, putrescine, cadaverine, histamine, tyramine, spermidine) in food samples. Parameters affecting the performance of the in situ derivatization process such as type of extraction solvent, temperature, extraction time, stirring speed and salt addition were studied and optimized. Under the optimized conditions (extraction solvent, dihexyl ether; acceptor phase, 0.1M HCl; extraction time, 30 min; extraction temperature, 26 degrees C; without addition of salt), enrichment factors varying from 47 to 456 were achieved. Good linearity of the analytes was obtained over a concentration range of 0.1-5 microg mL(-1) (with correlation coefficients of 0.9901-0.9974). The limits of detection and quantification based on a signal-to-noise ratio of 3-10, ranged from 0.0075 to 0.030 microg mL(-1) and 0.03 to 0.10 microg mL(-1), respectively. The relative standard deviations based on the peak areas for six replicate analysis of water spiked with 0.5 microg mL(-1) of each biogenic amine were lower than 7.5%. The method was successfully applied to shrimp sauce and tomato ketchup samples, offering an interesting alternative to liquid-liquid extraction and solid phase extraction for the analysis of biogenic amines in food samples.

Matched MeSH terms: Chromatography, High Pressure Liquid/instrumentation; Chromatography, High Pressure Liquid/methods*
Alpha-tocopherol content in 62 edible tropical plants

Ching LS, Mohamed S

J Agric Food Chem, 2001 Jun;49(6):3101-5.
PMID: 11410015

Vitamin E was determined by the high-performance liquid chromatography (HPLC) method. All the plants tested showed differences in their alpha-tocopherol content and the differences were significant (p < 0.05). The highest alpha-tocopherol content was in Sauropus androgynus leaves (426.8 mg/kg edible portion), followed by Citrus hystrix leaves (398.3 mg/kg), Calamus scipronum (193.8 mg/kg), starfruit leaves Averrhoa belimbi (168.3 mg/kg), red pepper Capsicum annum (155.4 mg/kg), local celery Apium graveolens (136.4 mg/kg), sweet potato shoots Ipomoea batatas (130.1 mg/kg), Pandanus odorus (131.5 mg/kg), Oenanthe javanica (146.8 mg/kg), black tea Camelia chinensis (183.3 mg/kg),papaya Carica papaya shoots (111.3 mg/kg), wolfberry leaves Lycium chinense (94.4 mg/kg), bird chili Capsicum frutescens leaves (95.4 mg/kg), drumstick Moringa oleifera leaves (90.0 mg/kg), green chili Capsicum annum (87 mg/kg), Allium fistulosum leaves (74.6 mg/kg), and bell pepper Capsicum annum (71.0 mg/kg). alpha-Tocopherol was not detected in Brassica oleracea, Phaeomeria speciosa, Pachyrrhizus speciosa, Pleurotus sajor-caju, and Solanum melongena.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods
Improved high performance liquid chromatographic analysis of omeprazole in human plasma

Yuen KH, Choy WP, Tan HY, Wong JW, Yap SP

J Pharm Biomed Anal, 2001 Feb;24(4):715-9.
PMID: 11272330

A simple high-performance liquid chromatographic method was developed for the determination of omeprazole in human plasma. Omeprazole and the internal standard, chloramphenicol, were extracted from alkalinized plasma samples using dichloromethane. The mobile phase was 0.05 M Na2HPO4-ACN (65:35, v/v) adjusted to pH 6.5. Analysis was run at a flow rate of 1.0 ml/min at a detection wavelength of 302 nm. The method was specific and sensitive with a detection limit of 2.5 ng/ml at a signal-to-noise ratio of 4:1. The limit of quantification was set at 5 ng/ml. The calibration curve was linear over a concentration range of 5-1280 ng/ml. Mean recovery value of the extraction procedure was about 96%, while the within and between day coefficient of variation and percent error values of the assay method were all less than 14%.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
Determination of four lignans in Phyllanthus niruri L. by a simple high-performance liquid chromatography method with fluorescence detection

Murugaiyah V, Chan KL

J Chromatogr A, 2007 Jun 22;1154(1-2):198-204.
PMID: 17418855 DOI: 10.1016/j.chroma.2007.03.079

A new and simple analytical method using HPLC with fluorescence detection was developed for the simultaneous determination of four lignans (phyllanthin, hypophyllanthin, phyltetralin and niranthin) in Phyllanthus niruri L. plant samples. Optimal separation was achieved with an isocratic mobile phase consisting of acetonitrile-water (55:45 v/v). The method recorded limits of detection (S/N=5) for phyllanthin at 0.61 ng/mL, hypophyllanthin at 6.02 ng/mL, phyltetralin at 0.61 ng/mL and niranthin at 1.22 ng/mL, being 80, 8, 80 and 40 times, respectively, lower when compared with those derived using HPLC-UV detection. The limits of quantification (S/N=12) were 4.88 ng/mL for phyllanthin and phyltetralin, 9.76 ng/mL for niranthin and 24.4 ng/mL for hypophyllanthin showing 40, 8 and 20 times, respectively, lower than those from the UV detection method. The within-day and between-day accuracy for the four lignans were between 98.1% and 102.9% while their precision values were below 2.2%. The mean recovery was between 92.5% and 110.1%. The method was then successfully applied for the quantification of lignans in P. niruri plant samples. The highest amount of lignans was found in the leaves followed by fruits, branches and stem, whilst the roots have the least amount of lignans.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
Fulltext Fast and Sensitive HPLC-ESI-MS/MS Method for Etoricoxib Quantification in Human Plasma and Application to Bioequivalence Study

Loh GOK, Wong EYL, Tan YTF, Heng SC, Saaid M, Cheah KY, et al.

Molecules, 2022 Sep 04;27(17).
PMID: 36080473 DOI: 10.3390/molecules27175706

Etoricoxib is a non-steroidal anti-inflammatory drug (NSAID) used to treat pain and inflammation. The objective of the current study was to develop a sensitive, fast and high-throughput HPLC-ESI-MS/MS method to measure etoricoxib levels in human plasma using a one-step methanol protein precipitation technique. A tandem mass spectrometer equipped with an electrospray ionization (ESI) source operated in a positive mode and multiple reaction monitoring (MRM) were used for data collection. The quantitative MRM transition ions were m/z 359.15 > 279.10 and m/z 363.10 > 282.10 for etoricoxib and IS. The linear range was from 10.00 to 4000.39 ng/mL and the validation parameters were within the acceptance limits of the European Medicine Agency (EMA) and Food and Drug Analysis (FDA) guidelines. The present method was sensitive (10.00 ng/mL with S/N > 40), simple, selective (K prime > 2), and fast (short run time of 2 min), with negligible matrix effect and consistent recovery, suitable for high throughput analysis. The method was used to quantitate etoricoxib plasma concentrations in a bioequivalence study of two 120 mg etoricoxib formulations. Incurred sample reanalysis results further supported that the method was robust and reproducible.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods
Frying performance of palm-based solid frying shortening

Omar MN, Nor-Nazuha MN, Nor-Dalilah MN, Sahri MM

Pak J Biol Sci, 2010 Mar 15;13(6):298-302.
PMID: 20506718

In order to evaluate the frying performance of palm-based solid frying shortening against standard olein, the fresh potato chips were fried in both frying media using an open fryer. After frying the chips for 40 h in an open batch fryer, it was found that the frying quality of palm-based solid frying shortening was better than standard palm olein in terms of Free Fatty Acid (FFA) values, Total Polar Content (TPC) and Total Polymeric Material (TPM). Solid shortening gave FFA, TPC and TPM values of 0.7, 15.3 and 2.67%, respectively, whilst standard palm olein gave values for FFA, TPC and TPM of 1.2, 19.6 and 3.10%, respectively. In terms of sensory mean scores, sensory panelists preferred the color of potato chips fried in solid shortening on the first day of frying, while on the third and fifth day of frying there were no significant differences (p < 0.05) in the sensory scores of fried products in both frying mediums. However, on the fifth day of frying, panelists gave higher scores in terms of taste, flavor and crispness for potato chips fried in solid shortening. These findings show that the palm-based solid shortening is better than palm olein when used for deep fat frying in terms of FFA values, total polar content and total polymeric material, especially for starch-based products such as potato chips. The result also shows that, in terms of sensory mean scores, after frying for 40 h, the sensory panelists gave higher scores in terms of taste, flavor and crispiness for potato chips fried in palm-based solid shortening.

Matched MeSH terms: Chromatography, High Pressure Liquid
Fulltext Caffeine and theobromine levels in chocolate couverture and coating products

Ramli N, Abdul Rahman S, Hassan O, Mohd Yatim A, Said M, Lim LS, et al.

Malays J Nutr, 2000 Mar;6(1):55-63.
PMID: 22692392

Thirty-two samples of chocolate products were analysed by HPLC for caffeine and theobromine contents. Defatted residues of samples were extracted with 80% aqueous acetone. After extraction into boiling water, the methylxanthines were identified and quantified with the use of μ-Bondapak column and mobile phase of methanol:water:acetic acid (20:79:1). Levels of caffein and theobromine in 32 samples of chocolate products averaged 0.62-1.14 mg/g and 0.026-0.153 mg/g respectively. Mean values for theobromine and caffeine content for chocolate coating were 0.82 and 0.07 mg/g respectively. The chocolate coating made from fat substitute had theobromine and caffeine levels ranging from 0.36-0.70 mg/g and 0.027-0.061 mg/g respectively, with mean values of 0.49 mg theobromine/g and 0.039 mg caffeine/g. In local chocolate, the mean theobromine and caffeine levels respectively were 0.72 mg/g and 0.04 mg/g in milk chocolate, and 0.85 mg/g and 0.06 mg/g in dark chocolate. Meanwhile, for imported chocolate, the mean theobromine and caffeine levels respectively were 1.05 mg/g and 0.12 mg/g in dark chocolate; 0.76 mg/g and 0.04 mg/g in milk chocolate; and 0.74 mg/g and 0.03 mg/g in white chocolate. Compared with the local chocolates, imported chocolates had higher levels of theobromine and caffeine at 1.141 mg/g and 0.1533mg/g. The average theobromine and caffeine concentrations in local chocolate were 0.082mg/g and 0.066mg/g. Theobromine concentration in chocolate samples is within the range of 0.62mg/g-1.141mg/g and the range of caffeine concentration is 0.026mg/g-0.153mg/g respectively. Bittersweet chocolates were found to have higher theobromine and caffeine concentrations than normal sweet chocolates and milk chocolates.

Matched MeSH terms: Chromatography, High Pressure Liquid
Fulltext Supercritical fluid extraction of bioactive flavonoid from Strobilanthes crispus (pecah kaca) and its comparison with solvent extraction

Liza, M.S., Abdul Rahman, R., Mandana, B., Jinap, S., Rahmat, A., Zaidul, I.S.M., et al.

International Food Research Journal, 2012;19(2):503-508.
MyJurnal

Supercritical carbon dioxide extraction (SC-CO2) of bioactive flavonoid from Strobilanthes crispus (Pecah Kaca) was performed to study the effects of various parameters such as pressure, temperature and dynamic extraction time on the yield and composition of bioactive flavonoid. The results were also compared with those obtained by conventional Soxhlet extraction in lab conditions. The results from SFE showed that the effect of extraction variables on extraction yields decreased in the following order: pressure, temperature and dynamic extraction time. The extraction pressure played a dominant role in the yield of the sample while the effect of time could be ignored. This study also revealed that both Soxhlet extraction and SC-CO2 extraction can be used to obtain flavonoid compound. Under the optimum conditions, the highest bioactive flavonoid compound content was obtained at 3.98% and eight flavonoid compounds were identified by HPLC.

Matched MeSH terms: Chromatography, High Pressure Liquid
Kesan kepekatan asid performik terhadap pengepoksidaan minyak sawit olein

Darfizzi Derawi, Jumat Salimon

Sains Malaysiana, 2011;40:1123-1127.

Kajian pengoptimuman tindak balas pengepoksidaan minyak sawit olein (POo) dengan menggunakan mangkin asid performik (HCOOOH) telah dijalankan. Kesan tindak balas terhadap nisbah kepekatan HCOOH : H2O2 dan masa tindak balas telah dikaji pada suhu 45oC. Kandungan oksigen oksirana (OOC) optimum sebanyak 3.61% diperoleh dengan menggunakan nisbah mol 1 : 5 : 2 pada 150 min dan sebanyak 96.5% penukaran dapat dicapai. Hasil tindak balas adalah sebanyak 91.3%. Puncak kromatografi cecair berprestasi tinggi (HPLC) bagi minyak sawit olein terepoksida (EPOo) telah berubah sepenuhnya berbanding puncak HPLC POo. Spektrum transformasi Fourier infra-merah (FTIR) telah menunjukkan kehadiran puncak ikatan gelang oksirana pada 844 cm-1.

Matched MeSH terms: Chromatography, High Pressure Liquid
Fulltext Simple and sensitive method for the analysis of ketorolac in human plasma using high-performance liquid chromatography

Muralidharan S, Jayaraja Kumar K, Parasuraman S

J Young Pharm, 2013 Sep;5(3):98-101.
PMID: 24396250 DOI: 10.1016/j.jyp.2013.06.007

To develop a simple and sensitive method of ketorolac in drug free human plasma using high-performance liquid chromatographic (HPLC).

Matched MeSH terms: Chromatography, High Pressure Liquid
Evaluation of role of HPLC (Merits & Pitfalls), in the diagnosis of various hemoglobinopathies & thalassemic syndromes

Baig MA, Swamy KB, Baksh AD, Bahashwan A, Moshrif Y, Al Sawat A, et al.

Indian J Pathol Microbiol, 2021 8 4;64(3):518-523.
PMID: 34341263 DOI: 10.4103/IJPM.IJPM_709_20

Background: : HPLC is one of the most important tools for accurate diagnosis of hemoglobinopathies and thalassemias. The advantage of the HPLC system is the excellent resolution, reproducibility &quantification of several normal and abnormal hemoglobin.
Results: BIO RAD Variant II analyzer was used. Sickle cell syndromes including double heterozygous states accounted for 56.13% of total cases. HbSS, HbS/β0-th, HbS/β+-th β-thal trait comprises 29%, 6.5%, 5.1%& 10% of total cases respectively with mean MCV (fl) = 84, 68,71,64 respectively. The Mean HbA2 for β-thal trait, HbE trait &HbE-β thal showed 5.1 ± 1.1, 19 ± 9 & 24 ± 8 respectively. HbF is increased in 8.6% case (excluding SC syndromes & β-thal disorders), of these 5.5% were infants & 12 cases of Aplastic Anemias. Peak P2 >7% (2.4% cases) was seen in uncontrolled diabetes mellitus which on quantification showed HbA1C = 8 ± 2.1 mmol/L.
Discussion: : HPLC in correlation with CBC parameters & family studies can aid in the diagnosis of majority of Hemoglobinopathies and thalassemic syndrome. The CBC & HPLC parameters of the present study are in good correlation with the research conducted by Tejinder Sing, RiouJ & Alla Joutovsky. Present study showed HPLC comprehensively characterizing HbS, A, A2, F, S, C, D from each other & was also applicable for the quantification of HbA1c for the monitoring of Diabetes Mellitus.
Conclusion: : The merits of HPLC are small quantity of sample required, economical, less TAT, accurate categorization of HbS, HbA2 & F. But one has to be aware of the limitations and problems associated with this method due to variant hemoglobin within the same retention windows. The present findings show HPLC as an excellent & powerful diagnostic tool for the direct identification of hemoglobin variants with a high degree of precision in the quantification of normal and abnormal hemoglobin fractions.

Matched MeSH terms: Chromatography, High Pressure Liquid/economics; Chromatography, High Pressure Liquid/methods*; Chromatography, High Pressure Liquid/standards*
Your mycotoxins in water paper

Paterson RRM, Buddie A

Environ Sci Pollut Res Int, 2019 05;26(13):13676.
PMID: 30357675 DOI: 10.1007/s11356-018-3544-3
Matched MeSH terms: Chromatography, High Pressure Liquid
Stability indicating HPLC-UV method for detection of curcumin in Curcuma longa extract and emulsion formulation

Syed HK, Liew KB, Loh GO, Peh KK

Food Chem, 2015 Mar 1;170:321-6.
PMID: 25306352 DOI: 10.1016/j.foodchem.2014.08.066

A stability-indicating HPLC-UV method for the determination of curcumin in Curcuma longa extract and emulsion was developed. The system suitability parameters, theoretical plates (N), tailing factor (T), capacity factor (K'), height equivalent of a theoretical plate (H) and resolution (Rs) were calculated. Stress degradation studies (acid, base, oxidation, heat and UV light) of curcumin were performed in emulsion. It was found that N>6500, T<1.1, K' was 2.68-3.75, HETP about 37 and Rs was 1.8. The method was linear from 2 to 200 μg/mL with a correlation coefficient of 0.9998. The intra-day precision and accuracy for curcumin were ⩽0.87% and ⩽2.0%, while the inter-day precision and accuracy values were ⩽2.1% and ⩽-1.92. Curcumin degraded in emulsion under acid, alkali and UV light. In conclusion, the stability-indicating method could be employed to determine curcumin in bulk and emulsions.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
Effect of deprotenizing agent and quantification of donepezil hydrochloride in human plasma

Liew KB, Peh KK, Fung Tan YT

Pak J Pharm Sci, 2014 Sep;27(5):1303-7.
PMID: 25176366

The effect of deprotenizing agents on recovery of donepezil hydrochloride in the development of a simple, rapid, selective and sensitive high performance liquid chromatography method for quantification of donepezil hydrochloride in human plasma was described. The deprotenizing agents were comprised of, perchloric acid, methanol, acetonitrile, chloroform and their mixtures. The chromatographic separation was carried out using reversed phase C18 column (Agilent Eclipse Plus C18) with UV detection at 268 nm. The mobile phase was comprised of 0.01 M potassium dihydrogen phosphate buffer, methanol and acetronitrile (50:30:20, v/v) adjusted to pH 2.7 with phosphoric acid (80%). A combination of perchloric acid and methanol gave a cleaner sample with a good recovery of donepezil hydrochloride of above 96%. The method showed intraday precision and accuracy in the range of 6.82% to 1.5% and 3.13% to 1.12% respectively, while interday precision and accuracy ranged between 1.06% to 4.71% and 13.01% to 6.43% respectively. The standard calibration curve was linear from 30ng/mL to 4000ng/mL, with a correlation coefficient of 0.9965±0.0034. The retention time of donepezil was 5.9 min with a run time of 7.0 min. The method can be applied to analyze large batch plasma samples in pharmacokinetic studies.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
A simple semi-preparative reversed-phase HPLC/PDA method for separation and quantification of glycyrrhizin in nine samples of Glycyrrhiza glabra root collected from different geographical origins

Basar N, Talukdar AD, Nahar L, Stafford A, Kushiev H, Kan A, et al.

Phytochem Anal, 2014 Sep-Oct;25(5):399-404.
PMID: 24585378 DOI: 10.1002/pca.2507

Glycyrrhiza glabra L. (Fabaceae), commonly known as 'liquorice', is one of the most popular ingredients in several traditional herbal medicinal preparations, and glycyrrhizin is the major glycoside present in this plant. The content of glycyrrhizin may vary among G. glabra samples collected from various geographical origins, which may affect the therapeutic efficacy. Thus, quantification of glycyrrhizin in G. glabra samples is important.

Matched MeSH terms: Chromatography, High Pressure Liquid*
Characteristic fingerprint based on gingerol derivative analysis for discrimination of ginger (Zingiber officinale) according to geographical origin using HPLC-DAD combined with chemometrics

Yudthavorasit S, Wongravee K, Leepipatpiboon N

Food Chem, 2014 Sep 1;158:101-11.
PMID: 24731320 DOI: 10.1016/j.foodchem.2014.02.086

Chromatographic fingerprints of gingers from five different ginger-producing countries (China, India, Malaysia, Thailand and Vietnam) were newly established to discriminate the origin of ginger. The pungent bioactive principles of ginger, gingerols and six other gingerol-related compounds were determined and identified. Their variations in HPLC profiles create the characteristic pattern of each origin by employing similarity analysis, hierarchical cluster analysis (HCA), principal component analysis (PCA) and linear discriminant analysis (LDA). As results, the ginger profiles tended to be grouped and separated on the basis of the geographical closeness of the countries of origin. An effective mathematical model with high predictive ability was obtained and chemical markers for each origin were also identified as the characteristic active compounds to differentiate the ginger origin. The proposed method is useful for quality control of ginger in case of origin labelling and to assess food authenticity issues.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
Validation of a HPLC method for determination of hydroxymethylfurfural in crude palm oil

Ariffin AA, Ghazali HM, Kavousi P

Food Chem, 2014 Jul 1;154:102-7.
PMID: 24518321 DOI: 10.1016/j.foodchem.2013.12.082

For the first time 5-hydroxymethyl-2-furaldehyde (HMF) was separated from crude palm oil (CPO), and its authenticity was determined using an RP-HPLC method. Separation was accomplished with isocratic elution of a mobile phase comprising water and methanol (92:8 v/v) on a Purospher Star RP-18e column (250mm×4.6mm, 5.0μm). The flow rate was adjusted to 1ml/min and detection was performed at 284nm. The method was validated, and results obtained exhibit a good recovery (95.58% to 98.39%). Assessment of precision showed that the relative standard deviations (RSD%) of retention times and peak areas of spiked samples were less than 0.59% and 2.66%, respectively. Further, the limit of detection (LOD) and LOQ were 0.02, 0.05mg/kg, respectively, and the response was linear across the applied ranges. The crude palm oil samples analysed exhibited HMF content less than 2.27mg/kg.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
Development and validation of an ion-pair chromatographic method for simultaneous determination of trans- and cis-urocanic acid in fish samples

Zare D, Muhammad K, Bejo MH, Ghazali HM

J Chromatogr A, 2012 Sep 21;1256:144-9.
PMID: 22885043 DOI: 10.1016/j.chroma.2012.07.083

Urocanic acid (UCA) has been reported to be a mast cell degranulator and has also been suggested as a complementary agent in implicated scombroid fish poisoning. In this research, a new method is described to extract, clean up and perform simultaneous ion-pair chromatographic analysis of trans- and cis-urocanic acid (UCA) in fish samples. UCA was extracted using 0.05 M HCl and protein was removed from the extract by precipitation with 10% trisodium citrate and 10% citric acid. The HPLC method that is developed showed a rapid, precise and sensitive method with short retention time for simultaneous separation of UCA isomers in fish samples. Estimation of trans- and cis-UCA in the muscle of Indian mackerel, tuna and sardine showed that, as expected, no cis-UCA existed in fish muscles and the highest concentration of trans-UCA was found in Indian mackerel with 118.8 mg kg(-1) while the highest concentrations of trans-UCA in tuna and sardine were 12.1 and 17.5 mg kg(-1), respectively.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
Fulltext A simple isocratic HPLC method for the simultaneous determination of sinensetin, eupatorin, and 3'-hydroxy-5,6,7,4'-tetramethoxyflavone in Orthosiphon stamineus extracts

Yam MF, Mohamed EA, Ang LF, Pei L, Darwis Y, Mahmud R, et al.

J Acupunct Meridian Stud, 2012 Aug;5(4):176-82.
PMID: 22898066 DOI: 10.1016/j.jams.2012.05.005

Orthosiphon stamineus extracts contain three flavonoids (3'-hydroxy-5,6,7,4'-tetramethoxyflavone, sinensetin, and eupatorin) as bioactive substances. Previous reported high performance liquid chromatography- ultraviolet (HPLC-UV) methods for the determination of these flavonoids have several disadvantages, including unsatisfactory separation times and not being well validated according to International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH) standard guidelines. A rapid, specific reversed-phase HPLC method with isocratic elution of acetonitrile: isopropyl alcohol: 20mM phosphate buffer (NaH(2)PO(4)) (30:15:55, v/v) (pH 3.5) at a flow-rate of 1ml/minute, a column temperature of 25°C, and ultraviolet (UV) detection at 340 nm was developed. The method was validated and applied for quantification of different types of O stamineus extracts and fractions. The method allowed simultaneous determination of 3'-hydroxy-5,6,7,4'-tetramethoxyflavone, sinensetin, and eupatorin in the concentration range of 0.03052-250 μg/ml. The limits of detection and quantification, respectively, were 0.0076 and 0.061 μg/ml for 3'-hydroxy-5,6,7,4'-tetramethoxyflavone, 0.0153 and 0.122 μg/ml for sinensetin and 0.0305 and 0.122 μg/ml for eupatorin. The percent relative standard deviation (% RSD) values for intraday were 0.048-0.368, 0.025-0.135, and 0.05-0.476 for 3'-hydroxy-5,6,7,4'-tetramethoxyflavone, sinensetin, and eupatorin, respectively, and those for intraday precision were 0.333-1.688, 0.722-1.055, and 0.548-1.819, respectively. The accuracy for intraday were 91.25%-103.38%, 94.32%-109.56%, and 92.85%-109.70% for 3'-hydroxy-5,6,7,4'-tetramethoxyflavone, sinensetin, and eupatorin, respectively, and those for interday accuracy were 97.49%-103.92%, 103.58%-104.57%, and 103.9%-105.33%, respectively. The method was found to be simple, accurate and precise and is recommended for routine quality control analysis of O stamineus extract containing the three flavonoids as the principle components in the extract.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*
A 4-hydroxy-N'-[(E)-(2-hydroxyphenyl)methylidene]benzohydrazide-based sorbent material for the extraction-HPLC determination of biogenic amines in food samples

Tameem AA, Saad B, Makahleh A, Salhin A, Saleh MI

Talanta, 2010 Sep 15;82(4):1385-91.
PMID: 20801345 DOI: 10.1016/j.talanta.2010.07.004

A sorbent material based on a newly synthesized hydrazone ligand, 4-hydroxy-N'-[(E)-(2-hydroxyphenyl)methylidene]benzohydrazide was prepared by immobilizing the ligand into a silica sol-gel matrix. The capability of the sorbent material for the extraction of seven biogenic amines (BAs), i.e., tryptamine (TRY), beta-phenylethylamine (PEA), putrescine (PUT), cadaverine (CAD), histamine (HIS), tyramine (TYR), and spermidine (SPD) was studied. Under the adopted conditions, the sorbent showed good selectivity towards PUT, CAD, HIS and SPD (% extraction (%E)>96) while %E for TYR, TRY and PEA were 82.0, 78.9 and 46.4%, respectively. The sorbent could be used up to six extraction cycles for SPD, CAD and PUT and was applied to the determination of food samples ("budu", ketchup, orange juice, soy sauce) that were spiked with 20 mg L(-1) of the BAs. The extracted analytes were derivatized with dansyl chloride before the HPLC determination. With the exception of HIS and TYR in "budu" sample, reasonable recoveries were found for the other analytes in all the tested food samples.

Matched MeSH terms: Chromatography, High Pressure Liquid/methods*

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