Determination of Fucoxanthin in Bloom-Forming Macroalgae by HPLC–UV

Abstract Fucoxanthin is a carotenoid natural product with extensive biological activities and offers a variety of health benefits. Brown algae and diatoms are known producers of this compound as an important component of their light-harvesting complexes. Considering its important function in algal photosynthesis, we assume that the massive biomass from macroalgal blooms is potential bioresources of this compound. Accordingly, a high-performance liquid chromatography–ultra-violet (HPLC–UV) method was developed and validated for quantitation of fucoxanthin in bloom-forming macroalgal species from coastal waters of north China. The linear regression was acquired with r = 0.9991. The precisions were evaluated by intra- and inter-day tests, and the relative standard deviation (RSD) values were within the range of 0.59 and 2.30%, respectively. The recoveries for the method were observed over the range of 99.3–100.4% with RSD values < 2.6%. Our results showed that fucoxanthin occurs in all the tested algae including red and green algal species, which are not generally considered as fucoxanthin producers. Application of HPLC–time-of-flight mass spectrometry for the qualitative analysis further confirmed the production of fucoxanthin in these species. The developed method provided an insight into the potential of the macroalgal biomass commercial production of fucoxanthin.

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Quantification of Saponins in Asparagus racemosus by HPLC-Q-TOF-MS/MS

Natural Product Communications ◽

10.1177/1934578x1701200103 ◽

2017 ◽

Vol 12 (1) ◽

pp. 1934578X1701200 ◽

Cited By ~ 1

Author(s):

Churanya Onlom ◽

Nitra Nuengchamnong ◽

Watoo Phrompittayarat ◽

Waraporn Putalun ◽

Neti Waranuch ◽

...

Keyword(s):

Quality Control ◽

High Performance ◽

Dry Weight ◽

Asparagus Racemosus ◽

Bioactive Constituents ◽

Traditional Medicines ◽

Flight Mass Spectrometry ◽

Relative Standard ◽

The One ◽

Tof Ms

Asparagus racemosus Willd. or Shatavari (Asparagaceae family) is an important medicinal plant in Ayurvedic medicine as a rejuvenate for women. A method for quantitative analysis of saponin glycosides bioactive constituents in A. racemosus is reported. A high performance liquid chromatography quadrupole time of flight mass spectrometry (HPLC-Q-TOF-MS/MS) method was developed and validated for simultaneous determination of five saponin glycosides, asparacoside, shatavarin IX, shatavarin IV, asparanin A and shatavarin V in A. racemosus extracted with 70% MeOH. The method was validated through intra-and inter-day precision, with the relative standard deviation (RSD) less than 6%, limits of detection (LOD) and limits of quantification (LOQ) <10 and 50 ng, respectively. Overall recoveries ranged from 95% to 105%, with RSD ranging from 0.7% to 4.5%. The method was applied to saponin glycoside contents in the leaves, stems, and roots of A. racemosus sourced from different geographical locations, including four provinces in Thailand, and a sample from India. Saponin glycosides were detected predominantly in the roots, the part used in traditional medicines and these showed wide variations in saponin glycoside profiles from undetectable to 12 mg/g dry weight. The quality control of A. racemosus is crucial for reliable and predictable therapies and only methods like the one developed has the necessary flexibility, sensitivity, accuracy, and selectivity for reliable routine quality control.

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Chemical components and biological activities of two freshwater green algae from Ordu, Turkey / Türkiye’nin Ordu ilinden iki tatlı su yeşil alglerinin kimyasal bileşenleri ve biyolojik aktiviteleri

Turkish Journal of Biochemistry ◽

10.1515/tjb-2015-0042 ◽

2015 ◽

Vol 40 (6) ◽

Author(s):

Beyhan Taş ◽

Ömer Ertürk ◽

Özlem Yılmaz ◽

Melek Çol Ayvaz ◽

Emine Yurdakul Ertürk

Keyword(s):

Antimicrobial Activity ◽

Total Phenolic Content ◽

Phenolic Content ◽

Biological Activities ◽

Algal Species ◽

Acetone Extract ◽

Diethyl Ester ◽

Diffusion Method ◽

Total Phenolic ◽

Green Algal

AbstractObjective: Scientists are looking for new resources which have biological activities. The present study was planned to evaluate the antioxidant and antimicrobial activity of ethanol and acetone extracts, as well as the volatile compounds of two freshwater green algal species Spirogyra spp. and Zygnema stellinum (Vaucher) C. Agardh belonging to Zygnemaphyceae (Conjugatophyceae) obtained from Ordu University Campus wetlands.Methods: The extracts were tested in vitro for their antimicrobial effects using disc diffusion method. Total phenolic content and the antioxidative activity according to FRAP and DPPH methods of the extracts were also determined. The secondary metabolites from the investigated extracts were identified using GC-MS.Results: The extracts dramatically inhibited almost all tested microorganisms. The antimicrobial activity of the acetone extract of the Zygnema against C. albicans was found as more higher than positive control Nystatin. In accordance with antimicrobial activity, the highest total phenolic content was also determined in the presence of the acetone extract of the Zygnema. Furthermore the highest FRAP value and the lowest EC50 (mg/mL) value were calculated for the same extract. The main components of the all consisted of dimethyl and diethyl ester of 1,2-benzenedicarboxylic acid. However, the abundance of these metabolites in the extracts was not associated with antimicrobial or antioxidant activity. Biological activities of these algal species could be attributed to chemicals such as 1-Pentadecene and 1-Tetradecene which were present in smaller amounts.Conclusion: Investigated algal species can be evaluated to use in biotechnological applications such as food industry and medicine.

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An integrated targeted and untargeted approach for the analysis of ergot alkaloids in cereals using UHPLC – hybrid quadrupole time-of-flight mass spectrometry

World Mycotoxin Journal ◽

10.3920/wmj2015.1900 ◽

2015 ◽

Vol 8 (5) ◽

pp. 653-666 ◽

Cited By ~ 6

Author(s):

N. Arroyo-Manzanares ◽

J. Diana Di Mavungu ◽

V. Uka ◽

L. Gámiz-Gracia ◽

A.M. García-Campaña ◽

...

Keyword(s):

Mass Spectrometry ◽

High Performance ◽

Time Of Flight ◽

Ergot Alkaloids ◽

Good Precision ◽

Method Performance ◽

Analytical Strategy ◽

Flight Mass Spectrometry ◽

Detection And Identification ◽

Relative Standard

An ultra-high performance liquid chromatography hybrid quadrupole – time of flight (Q-TOF) mass spectrometry (MS) method is described for the simultaneous quantitative determination of common ergot alkaloids and the screening, detection and identification of unexpected (less studied or novel) members of this class of toxic fungal secondary metabolites. The employed analytical strategy involves an untargeted data acquisition (consisting of full scan TOF MS survey and information dependent acquisition MS/MS scans) and the processing of data using both targeted and untargeted approaches. Method performance characteristics for the quantitative analysis of 6 common ergot alkaloids i.e. ergometrine, ergosine, ergotamine, ergocornine, ergocristine, ergokryptine and their corresponding epimers in rye were comparable to those previously reported for triple-quadrupole (QqQ) MS/MS. The method limits of quantification (LOQ) were in the range from 3 to 19 μg/kg, and good linearity was observed for the different ergot alkaloids in the range from LOQ to 1000 μg/kg. Furthermore, the method demonstrated good precision (relative standard deviations at 50 μg/kg not higher than 14.6 and 16.2% for the intra-day and inter-day precision, respectively), and the trueness values at different concentration levels were all between 89 and 115%. The method was applied for the analysis of a set of 17 rye samples and demonstrated the presence of these ergot alkaloids in the range from <LOQ to 2,811 μg/kg. Further mining of the same data based on a ‘non-targeted peak finding’ algorithm and the use of full MS and MS/MS accurate mass data allowed the detection and identification of 19 ergot alkaloids that are commonly not included in most analytical methods using QqQ instruments. Some of these alkaloids are reported for the first time in naturally contaminated samples.

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A NEW HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SEPARATION AND SIMULTANEOUS QUANTIFICATION OF EPTIFIBATIDE AND ITS IMPURITIES IN PHARMACEUTICAL INJECTION FORMULATION

International Journal of Applied Pharmaceutics ◽

10.22159/ijap.2021v13i2.39895 ◽

2021 ◽

pp. 165-172

Author(s):

K. SRI GIRIJA ◽

BIKSHAL BABU KASIMALA ◽

VENKATESWARA RAO ANNA

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

High Performance ◽

Degradation Products ◽

Ultra Violet ◽

Hplc Method ◽

Chromatography Method ◽

Standard Drug ◽

Pharmaceutical Dosage Forms ◽

Relative Standard

Objective: The objective of the present study is to develop a stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for qualitative and quantitative determination of Eptifibatide and its impurities in bulk and pharmaceutical dosage forms. Methods: The chromatographic separation was carried on Phenomenex Luna C18 column (250 mm×4.6 mm; 5µ id) as stationary phase, methanol and phosphate buffer at pH 6.4 in the ratio of 65:45 (v/v) as mobile phase at flow rate of 1.0 ml/min, Ultra Violet (UV) detection was carried at the wavelength of 236 nm and the analysis was completed with a run time of 15 min. Results: In the developed conditions, the retention time of Eptifibatide and its impurities 1 and 2 were found to be 3.35, 4.93 and 8.18 min, respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability and robustness. Spiked recovery at 50%, 100% and 150% was carried for both standard and impurities and the acceptable % recovery of 98-102 was observed for Eptifibatide and both impurities studied and the % Relative standard deviation (RSD) in each spiked level was found to be less than 2. Stability tests were done through the exposure of the analyte solution to five different stress conditions i. e expose to 1N Hydrochloric acid (HCl), 1 N Sodium hydroxide (NaOH), 3% Hydrogen peroxide (H2O2), 80 °C temperature to UV radiation. In all the degradation conditions, standard drug Eptifibatide was detected along with both the impurities studied and the degradation products were successfully separated. In the formulation analysis, there is no other chromatographic detection of other impurities and formulation excipients. Conclusion: The developed method was found to be suitable for the quantification of Eptifibatide and can separate and analyse impurities 1 and 2.

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Detection Of Pendimethalin and Cypermetrin Residues in Locally Produced Tomato Using QuEChERS-HPLC Analysis

Nigerian Journal of Basic and Applied Sciences ◽

10.4314/njbas.v27i1.5 ◽

2020 ◽

Vol 27 (1) ◽

pp. 34-40

Author(s):

L.B. Abdulra’uf ◽

F.A. Adeyemo ◽

F.B. Atanda ◽

R. Lawal

Keyword(s):

Chromatographic Analysis ◽

High Performance ◽

Hplc Analysis ◽

Correlation Coefficients ◽

Ultra Violet ◽

Uv Detector ◽

Relative Standard ◽

Detector Method ◽

Maximum Residue Levels ◽

Residue Levels

This study investigated the levels of pendimethalin and cypermetrin residues in tomato sold in Malete market, Moro Local Government Area of Kwara State. Tomatoes were randomly collected from five different vendors in Malete market and analysis was performed using the QuEChERS (Quick, Easy Cheap, Effective, Rugged and Safe) method followed by chromatographic analysis using high performance liquid chromatography (HPLC) coupled to ultra-violet (UV) detector. Method validation of the study showed a linearity of the analytes which ranges from 5 – 500 μg/kg, with correlation coefficients greater than 0.999. The average recovery ranges from 75.6 to 111 % with relative standard deviation (RSD) from 2.74 to 9.03 %. The results indicated the presence of cypermethrin in analyzed samples at concentrations lower than the permissible maximum residue levels Keywords: Sample preparation, Pesticide residues, HPLC-UV, QuEChERS.

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Quantification of Pyrazinamide in Human Plasma by Validated High Performance Liquid Chromatography Method

10.53350/pjmhs2115102896 ◽

2021 ◽

Vol 15 (10) ◽

pp. 2896-2899

Author(s):

Waleed Arshad ◽

Naseem Saud Ahmad ◽

Abdul Muqeet Khan ◽

Iram Imran ◽

Qura- Tul-Ain ◽

...

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Human Plasma ◽

Mobile Phase ◽

High Performance ◽

Ultra Violet ◽

Chromatography Method ◽

Ultraviolet Detector ◽

Relative Standard ◽

Liquid Chromatography Method

Objective: To be able to accurately determine the quantity of Pyrazinamide (PZA) in different tablet preparations and human plasma using an Ultra violet detector equipped high performance liquid chromatography (HPLC). Study Design: Experimental study Place and Duration of Study: Department of Bioequivalence Studies, University of Veterinary and Animal Sciences Lahore and the Department of Pharmacology, University of Health Sciences, Lahore the from 1st April 2017 to 31st March 2018. Methodology: Two mobile phases were used, the first compromised of disodium hydrogen phosphate buffer having a pH of 6.8 and acetonitrile in the proportion of (95:5) and the second was a combination of aforesaid substances in equivalent proportion (50:50 v/v). The gradient for the first 5 min was exclusively Mobile phase “a” after which 5-6 min Mobile phase “b” was raised from 0 to 100% and was kept at 100% till the completion of the cycle. The flow of mobile phase was kept at 1000 µl/min. Determination of PZA was done using a ultraviolet detector at a wavelength of 238 nm. Amount of sample injected was 40 μl. Procedure was done by using Shizmadu Chromatographic System, Japan equipped with a SIL-20AC HT auto-sampler, SPD-M20A, CTO 20 AC, a LC-20AT VP pump, and CBM 20A controller unit. A C18 column was used as well. Results: Retention time of PZA was 6.1±2%. Precision was 0.46 to 2.20% relative standard deviation for intra assay and for inter assay we obtained 0.29 to 34.45% RSD for all quality control levels. The overall recovery of PZA was 96.75%. Conclusion: High selectivity for PZA was seen and no other spikes from drugs present in FDC regimen were observed at the time when PZA is detected in blank plasma samples Key words: Chromatography, High pressure liquid. Pyrazinamide. Tuberculosis

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Simultaneous Quantitation of Five Bioactive Ingredients in Raw and Processed Fallopia multiflora by Employing UHPLC-Q-TOF-MS

Journal of Chromatographic Science ◽

10.1093/chromsci/bmz035 ◽

2019 ◽

Vol 57 (7) ◽

pp. 618-624

Author(s):

Yi Tao ◽

Xiaoping Zhou ◽

Weidong Li ◽

Baochang Cai

Keyword(s):

High Performance ◽

Limit Of Detection ◽

Bioactive Components ◽

Limit Of Quantification ◽

Sample Handling ◽

Flight Mass Spectrometry ◽

Relative Standard ◽

Bioactive Ingredients ◽

Aqueous Formic Acid

Abstract Fallopia multiflora is used for treatment of premature graying hair and blood deficiency. In this study, a quantitative method was developed for determination of five bioactive components (emodin, 2,3,5,4′-tetrahydroxy-stilbene- 2-Ο-β-d-glucoside, emodin-8-O-β-d-glucopyranoside, ω-hydroxyemodin and kaempferol) in raw and processed F. multiflora by using ultra-high performance liquid chromatography (UHPLC)-quadrupole time-of-flight mass spectrometry-based method. The sample handling procedure was optimized. Chromatographic separation was carried out on a Thermo Syncronis AQ-C18 UHPLC column with mobile phase consisting of 0.01% aqueous formic acid and acetonitrile. The method was interrogated in terms of linearity, precision, stability and recovery tests. All calibration curves displayed good linearity (R2 > 0.9992). The limit of detection and limit of quantification of these components ranged from 0.01 to 0.03 μg/mL and from 0.03 to 0.07 μg/mL, respectively. The average recoveries of these components were from 98.2 to 102.9% with relative standard deviation values from 0.8 to 2.9% for F. multiflora. The developed method can be applied to quality control of raw and processed F. multiflora.

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Ultrasound Assisted Dispersive Solid Phase Microextraction of Thymol and Carvacrol in Pharmaceutical Products Using Graphene Oxide as an Adsorbent Prior to Analysis by High Performance Liquid Chromatography

Current Pharmaceutical Analysis ◽

10.2174/1573412915666190220102628 ◽

2020 ◽

Vol 16 (5) ◽

pp. 578-584

Author(s):

Parvin Abedi Ghobadloo ◽

Samin Hamidi ◽

Mahboob Nemati ◽

Fatemeh Soghra Jahed

Keyword(s):

High Performance Liquid Chromatography ◽

Graphene Oxide ◽

Liquid Chromatography ◽

Solid Phase Microextraction ◽

High Performance ◽

Solid Phase ◽

Detection System ◽

Ultra Violet ◽

Pharmaceutical Products ◽

Relative Standard

Background: Thymol and carvacrol are the most important dietary constituents in thyme species. These two active compounds are used for the standardization of pharmaceutical compounds. Objective: In this work, a simple and reliable ultrasonic assisted dispersive solid phase microextraction method (USA-DSPME) coupled with high performance liquid chromatography-ultra violet detection system was developed to determine thymol and carvacrol in pharmaceutical syrups. The efficiency of SPME sorbent was examined through several sorbents and finally Graphene Oxide (GO) was applied for extraction of the analytes. Method: The efficiency of GO was compared with three reduced forms of GO adsorbents as well. Several effective factors on the extraction performance were investigated. Results: Under the optimized conditions for the GO sorbent, inter and intra-day relative standard deviations (RSDs, n = 3) and the Limits of Detections (LODs) were lower than 5.0% and 0.02 μg/ml, respectively. Moreover, good linear ranges were observed in wide concentration ranges with R-squared larger than 0.9961 for both thymol and carvacrol. Conclusion: The present method is reliable and simple for determination of carvacrol and thymol in pharmaceutical products.

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Solidified floating organic droplet microextraction coupled with HPLC for rapid determination of trans, trans muconic acid in benzene biomonitoring

Scientific Reports ◽

10.1038/s41598-021-95174-5 ◽

2021 ◽

Vol 11 (1) ◽

Author(s):

Fatemeh Dehghani ◽

Fariborz Omidi ◽

Omidreza Heravizadeh ◽

Saeed Yousefinejad

Keyword(s):

High Performance ◽

Limit Of Detection ◽

Rapid Determination ◽

Ultra Violet ◽

Work Environments ◽

Fast Method ◽

Muconic Acid ◽

Relative Standard ◽

Central Composite

AbstractBenzene is one of the carcinogenic compounds in the work environments. Exposure assessment of benzene through biological monitoring is an acceptable way to accurately measure the real exposure in order to conducting the health risk assessment, but it is always complicated, laborious, time consuming and costly process. A new sensitive, simple, fast and environmental friendly method was developed for the determination of urinary metabolite of benzene, trans trans muconic acid (t,t-MA) by dispersive liquid–liquid micro extraction based on solidification of floating organic droplet coupled with high-performance liquid chromatography with ultra violet detector. Central composite design methodology was utilized to evaluate the effective factors on the extraction output of the target metabolite. The calibration curve was plotted in the concentration ranges of 0.02–5 µg mL−1. The precision and accuracy of the method were assayed via the relative standard deviation (RSD%) and relative recovery (RR%) using spiked samples with three replications. The RR% and RSD% of the optimized method were 86.9–91.3% and 4.3–6.3% respectively. The limit of detection (LOD) of the method was 0.006 µg mL−1. The level of t,t-MA in real samples was ranged from 0.54 to 1.64 mg/g creatinine. We demonstrated that t,t-MA can be extracted and determined by an inexpensive, simple and fast method.

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Optimasi dan Validasi Metode Kromatografi Cair Kinerja Tinggi untuk Menetapkan Kadar Asam Klorogenat dalam Ekstrak Etanol Daun Yakon (Smallanthus sonchifolius (Poepp. & Endl.) H. Robinson)

ALCHEMY Jurnal Penelitian Kimia ◽

10.20961/alchemy.16.1.28952.66-76 ◽

2020 ◽

Vol 16 (1) ◽

pp. 66

Author(s):

Zuhelmi Aziz ◽

Liliek Nurhidayati ◽

Syamsudin Abdillah ◽

Nancy Dewi Yuliana ◽

Partomuan Simanjuntak

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Formic Acid ◽

Chlorogenic Acid ◽

High Performance ◽

Biological Activities ◽

Hplc Method ◽

Good Precision ◽

Smallanthus Sonchifolius ◽

Relative Standard

Yakon merupakan tanaman yang dapat digunakan untuk pengobatan dan kebutuhan pangan. Salah satu kandungan zat berkhasiat dalam daun yakon adalah asam klorogenat. Asam klorogenat diketahui memiliki aktifitas sebagai antioksidan, antikanker dan antidiabetes. Penentuan kadar asam klorogenat dalam matriks yang kompleks diperlukan metode yang selektif dengan ketelitian dan ketepatan yang baik. Pada penelitian ini dilakukan optimasi dan validasi metode kromatografi cair kinerja tinggi (KCKT) fase balik untuk penetapan kadar asam klorogenat. Ekstrak dibuat secara ultrasonikasi menggunakan pelarut etanol 95%. Kondisi optimum diperoleh menggunakan fase gerak asam format 0,1% dalam asetonitril–asam format 0,1% dalam air (gradien); fase diam oktadesilsilan (C18) pada suhu 30 ºC dan detektor UV pada panjang gelombang 328 nm. Metode KCKT ini memberikan hasil yang memiliki ketelitian yang tinggi dengan simpangan baku relatif 0,79% dan ketepatan yang baik dengan perolehan kembali 97,50%. Kadar asam klorogenat yang diperoleh dalam ekstrak etanol 95% daun yakon sebesar 1,02%. Optimization and Validation of High Performance Liquid Chromatography Methods for Determination of Chlorogenic Acid Levels in Ethanol Extracts of Yakon Leaves (Smallanthus sonchifolius (Poepp. & Endl.) H. Robinson). Yacon is a plant that can be used for medication and food needs. One of the bioactive compounds of yacon leaves is chlorogenic acid. Chlorogenic acid has various biological activities, such as antioxidant, anticancer and antidiabetic activities. To determine the chlorogenic acid in such complex matrix, such selective methods with good precision and acuracy are required. In this study, the optimization and validation of reverse phase high performance liquid chromatography (HPLC) method for chlorogenic acid determination were performed. The extract was prepared by ultrasonication in 95% ethanol.The optimized condition for HPLC obtained was by using mobile phase 0.1% formic acid in acetonitrile – 0.1% formic acid in water with gradient elution, stationary phase octadesylsilane (C18) at 30 oC and UV detector at of 328 nm. The result showed that HPLC method had high precicion with relative standard deviation of 0.79% and high accuracy with recovery of 97.50%. The chlorogenic acid in the ethanol 95% extract of Yacon leaves was 1,02%.<div> </div>

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