Development and Validation of a GC-MS Method for the Analysis of Homogentisic Acid in Strawberry Tree (Arbutus unedo L.) Honey

2017 ◽  
Vol 100 (4) ◽  
pp. 889-892 ◽  
Author(s):  
Irena Brčić Karačonji ◽  
Karlo Jurica
Keyword(s):  
Homogentisic Acid ◽  
Arbutus Unedo ◽  
Liquid Liquid Extraction ◽  
Strawberry Tree ◽  
Routine Monitoring ◽  
Average Accuracy ◽  
Reliable Performance ◽  
Extraction Solvents ◽  
Development And Validation

Abstract To confirm the botanical origin of strawberry tree (Arbutus unedo L.) honey, a liquid–liquid extraction followed by GC-MS method was developed for the quantitative determination of homogentisic acid (HGA), the main phenolic compound in this honey. Different parameters affecting extraction, such as the type and volume of extraction solvents, pH of the solution, and amount of salt, were optimized. The method showed good linearity (r2 = 0.9990) over the tested concentration range (50–500 mg/kg) and a low LOD (0.3 mg/kg). Precision expressed as RSD was <7%. The average accuracy was 95%. The optimized method was applied for determining the HGA content in strawberry tree honey samples from Croatia. The HGA content in analyzed samples (n = 7) ranged from 245.1 to 485.9 mg/kg. The proposed method provided reliable performance and can be easily implemented for the routine monitoring of HGA in strawberry tree honey in order to assure honey QC.

Direct chromatographic methods for the rapid determination of homogentisic acid in strawberry tree (Arbutus unedo L.) honey

2005 ◽  
Vol 1090 (1-2) ◽  
pp. 76-80 ◽  
Author(s):  
Roberta Scanu ◽  
Nadia Spano ◽  
Angelo Panzanelli ◽  
Maria I. Pilo ◽  
Paola C. Piu ◽  
...  
Keyword(s):  
Rapid Determination ◽  
Homogentisic Acid ◽  
Arbutus Unedo ◽  
Chromatographic Methods ◽  
Strawberry Tree

Determination of Phenolic Contents, Antioxidant and Antibacterial Activities of Strawberry Tree (Arbutus unedo L.) Leaf Extracts

2016 ◽  
Vol 14 (3) ◽  
pp. 1-10 ◽  
Author(s):  
Abdelhakim Bouyahya ◽  
Naima Moussaoui ◽  
Jamal Abrini ◽  
Youssef Bakri ◽  
Nadia Dakka
Keyword(s):  
Antibacterial Activities ◽  
Leaf Extracts ◽  
Arbutus Unedo ◽  
Phenolic Contents ◽  
Strawberry Tree

Liquid–Solid Sample Preparation Followed by Headspace Solid-Phase Microextraction Determination of Multiclass Pesticides in Soil

2012 ◽  
Vol 95 (5) ◽  
pp. 1331-1337 ◽  
Author(s):  
Rada D Ðurović ◽  
Tijana M Ðorðević ◽  
Ljiljana R Šantrić
Keyword(s):  
Sample Preparation ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Extraction Procedure ◽  
Soil Samples ◽  
Optimum Number ◽  
Headspace Solid Phase Microextraction ◽  
Extraction Solvents ◽  
Development And Validation

Abstract This paper describes development and validation of a multiresidue method for the determination of five pesticides (terbufos, prochloraz, chloridazon, pendimethalin, and fluorochloridone) belonging to different pesticide groups in soil samples by GC/MS, followed by its application in the analysis of some agricultural soil samples. The method is based on a headspace solid-phase microextraction method. Microextraction conditions, namely temperature, extraction time, and NaCl content, were tested and optimized using a 100 μm polydimethylsiloxane fiber. Three extraction solvents [methanol, methanol–acetone (1 + 1, v/v), and methanol–acetone–hexane (2 + 2 + 1, v/v/v)] and the optimum number of extraction steps within the sample preparation stage were optimized for the extraction procedure. LOD values for all the studied compounds were less than 12 μg/kg. Recovery values for multiple analyses of soil samples fortified at 30 μg/kg of each pesticide were higher than 64%. The method was proven to be repeatable, with RSD lower than 15%.

SENSITIVE BIO ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF VENETOCLAX IN HUMAN PLASMA BY LC-ESI-MS/MS

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (06) ◽  
pp. 32-38
Author(s):  
H. Potluri ◽  
Keyword(s):  
Human Plasma ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Liquid Liquid Extraction ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Mode ◽  
Method Development And Validation ◽  
Development And Validation

A specific and sensitive method of liquid chromatography–tandem mass spectrometry was demonstrated for the experimental determination of venetoclax in human plasma utilising venetoclax-D8 as an internal standard. The column Xbridge C18, 50 × 4.6mm, 5 µm was used for attaining chromatographic separation by utilising 10mM ammonium formate and methanol as isocratic mobile phase in the composition ratio of 20:80 (V/V). The flow-rate selected was 0.7ml/min. Venetoclax and venetoclax-D8 are identified in multiple reaction monitoring (MRM) positive mode with proton adducts at m/z 869.53 →553.21 and m/z 877.14 → 553.23, respectively. For the successful extraction of drug as well as internal standard, liquid-liquid extraction technique was efficiently utilised. The developed technique was established in a linear concentration range of 5.0-5000.0 pg/ml along with correlation coefficient (r2) of 0.9994. Intra and inter-day precisions were found to be 0.7 to 1.90% and 0.7 to 2.0 % for venetoclax and venetoclax-D8, respectively. Accuracy was found to be within 98.6 to 101.99% and 99.17 to 101.14 % for venetoclax and venetoclax-D8, respectively. It was observed that throughout the bench top studies, post-operative stability studies and freeze-thawing cycles, venetoclax retained stability.

Analytical method development and validation studies for estimation of anti-psychotic drug (Olanzapine)

2021 ◽  
Vol 7 (2) ◽  
pp. 127
Author(s):  
Renuka Manjunath ◽  
Deepak Kumar Jha
Keyword(s):  
Method Development ◽  
Anti Psychotic ◽  
Liquid Liquid Extraction ◽  
Ether Extraction ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Limit Mode ◽  
New Strategies ◽  
Butyl Methyl Ether

<p class="abstract"><strong>Background:</strong> Various sophisticated strategies have been raised in conformity with permit the fast separation and quantification about clue aspects concerning complex mixtures of biological matrix. These needs underscored the necessary of analytical instrumentation and the creation of new strategies.</p><p class="abstract"><strong>Methods:</strong> A rapid, accurate, precise, and simple UV then LC-MS/MS analytical methods has been flourished for the determination of Olanzapine (OLZ) in tablet formulation.  </p><p class="abstract"><strong>Results:</strong> Chromatographic separation was conducted out on a Phenomenex 250×4.60 mm with an isocratic mobile phase consisting formic acid of 0.1% v/v in Methanol and water at a ratio regarding 92:08v/v and an aggregation run time of 2.5 min. The plasma Olanzapine concentrations were quantified the use of SCIEX API 3000 LC-MS/MS provision geared up along electro spray ionization cleft into the multiple reaction limit mode at m/z 313.4 to 256.3 for Olanzapine; and m/z 327.1 to 270.0 for clozapine respectively. Calibration requirements were organized into the range 5 ng/ml in conformity with 1000 ng/ml for Olanzapine. The effects had been unique and reproducible with the samples prepared by way of liquid-liquid extraction method using Tert-butyl methyl ether extraction in the course of approach improvement trials.</p><p class="AT"><strong>Conclusions:</strong> The novelty on its technique entails the improvement and validation by means of the usage of some quadrant easy pattern decontamination approach and the most sensitive technique with shortest analysis time.</p>

BIOANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF MEMANTINE HYDROCHLORIDE BY SPECTROFLUORIMETRIC METHOD USING OPA Β-MERCAPTOETHANOL AS DERIVATIZING AGENT

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (09) ◽  
pp. 12-16
Author(s):  
C. B Patel ◽  
◽  
C. S. Kothari ◽  
N. R Patel ◽  
O Sherikar
Keyword(s):  
Human Plasma ◽  
Method Development ◽  
High Recovery ◽  
Synchronous Mode ◽  
Liquid Liquid Extraction ◽  
Spectrofluorimetric Method ◽  
Derivatizing Agent ◽  
Method Development And Validation ◽  
Development And Validation

A new, simple, accurate, sensitive and specific bioanalytical spectrofluorimetric method was developed and validated for estimation of memantine hydrochloride (MEM) in human plasma. Estimation of MEM in human plasma was done by spiked human plasma studies. Extraction of MEM from human plasma was carried out using 5% trichloroacetic acid for protein precipitation followed by liquid-liquid extraction with 5% IPA in n-hexane. For spectrofluorimetric estimation delta value 65 applied in synchronous mode (medium sensitivity mode) and fluorescence intensity was measured at 420 nm. Developed method was found linear to be in the concentration range of 50-300 ng/mL with correlation coefficient (R2) 0.9951. Percentage recovery was found to be 77.85-83.68% for MEM. High recovery shows that the method is free from the interference from plasma constituents. Hence, proposed method can be used for estimation of MEM in routine quality control laboratories for quantitative determination of MEM in bulk as well as in human plasma. Further it can also be used to determine plasma MEM concentration in drug monitoring or in pharmacokinetic investigations.

scholarly journals Development and Validation of a LC/MS/MS Method for the Determination of Duloxetine in Human Plasma and Its Application to Pharmacokinetic Study

2012 ◽  
Vol 9 (2) ◽  
pp. 899-911 ◽  
Author(s):  
D. Chandrapal Reddy ◽  
A. T. Bapuji ◽  
V. Surayanarayana Rao ◽  
V. Himabindu ◽  
D. Rama Raju ◽  
...  
Keyword(s):  
Human Plasma ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Pharmacokinetic Parameters ◽  
Liquid Liquid Extraction ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Edta Plasma ◽  
Development And Validation

A selective, high sensitive and high throughput liquid chromatography-tandem mass spectrometry (LC-ESI-MS/MS) method has been developed and validated for the chromatographic separation and quantitation of duloxetine in human EDTA plasma using fluoxetine (IS) as an internal standard. Analyte and IS were extracted from human plasma by liquid-liquid extraction using MTBE-n Hexane (80:20).The eluted samples were chromatographed on X-terra RP8 (50 mmx4.6 mm, 5 μm particle size) column by using mixture of 30 mM ammonium formate (pH-5.0±0.05) and acetonitrile as an isocratic mobile phase at a flow rate of 0.40 mL/min and analyzed by mass spectrometer in the multiple reaction monitoring (MRM) using the respective m/z 298.08→154.0 for duloxetine and 310.02→148.07 for IS. The linearity of the response/ concentration curve was established in human plasma over the concentration range 0.100-100.017 ng/mL. The lower detection limit (LOD,S/N>3) was 0.04 ng/mL and the lower limit of quantization (LOQ,S/N>10) was 0.100 ng/mL. This LC-MS/MS method was validated with Intra-batch and Inter-batch precision of 5.21-7.02. The Intra-batch and Inter-batch accuracy was 97.14-103.50 respectively. Recovery of duloxetine in human plasma is 80.31% and ISTD recovery is 81.09%. The main pharmacokinetic parameters were Tmax(hr) = (7.25±1.581), Cmax(ng/mL) (44.594±18.599), AUC0→t, = (984.702±526.502) and AUC0→∞, (1027.147±572.790) respectively.

scholarly journals Development and Validation of an HPLC/MS/MS Method for the Determination of Sufentanil and Morphine in Human Plasma

2011 ◽  
Vol 94 (1) ◽  
pp. 136-142 ◽  
Author(s):  
Josélia Larger Manfio ◽  
Verônica Jorge Santos ◽  
Vera Lúcia Lanchote ◽  
Luciana M Santos ◽  
Maria José C Carmona ◽  
...  
Keyword(s):  
Ammonium Acetate ◽  
Internal Standard ◽  
Triple Quadrupole Mass Spectrometer ◽  
Selective Reaction ◽  
Liquid Liquid Extraction ◽  
Electrospray Source ◽  
Positive Mode ◽  
Set Up ◽  
Development And Validation

Abstract A sensitive and fast HPLC/MS/MS method for measurement of sufentanil and morphine in plasma was developed and validated. A single liquid–liquid extraction in alkaline medium was used for the cleanup of plasma, and fentanyl was added as an internal standard (IS). The analyses were carried out using a C18 column and the mobile phase acetonitrile–5 mM ammonium acetate + 0.25% formic acid (70 + 30, v/v). The triple-quadrupole mass spectrometer equipped with an electrospray source in positive mode was set up in the selective reaction monitoring mode to detect precursor → product ion transition 387.0 &gt; 238.0, 285.7 &gt; 165.1, and 337.0 &gt; 188.0 for sufentanil, morphine, and IS, respectively. The method was linear in the 0.05 (LOQ) – 500 ng/mL range for sufentanil and 10 (LOQ) – 1000 ng/mL range for morphine. Good selectivity, linearity, precision, accuracy, and robustness were obtained for the HPLC/MS/MS method. The proposed method was successfully applied for the determination of sufentanil and morphine in patients undergoing cardiac surgery.

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