Rapid Determination of Amygdalin and its Novel Degradation Product in Plasma of Mice by SPE-HPLC

2013 ◽  
Vol 781-784 ◽  
pp. 83-88
Author(s):  
Chen Xi Wang ◽  
Yu Ping Li ◽  
Jun Chang ◽  
Bin Zhou ◽  
Xiao Han ◽  
...  
Keyword(s):  
Formic Acid ◽  
Extracellular Enzymes ◽  
Limit Of Detection ◽  
Rapid Determination ◽  
Gradient Elution ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
High Antitumor Activity ◽  
Set Up

Amygdalin was catalytic degraded by extracellular enzymes mixture from Aspergillus niger and a novel product, phenyl-(3,4,5-trihydroxy-6-methyl-tetrahydro-pyran-2-yloxy)-acetonitrile (PTMT), with high antitumor activity was identified and purified. To measured the Pharmacokinetic of amygdalin and its products, a simple and rapid SPE-HPLC method was set up. The analysis was performed on an Agilent HPLC system with a C18 ODS column (250 × 4.6 mm i.d.) by gradient elution with 0.05% formic acid in water and 0.05% formic acid in acetonitrile as the gradient mixtures. The flow rate was 1ml/min, the detection wavelength was 215 nm and the column temperature was kept at 25°C. The HPLC assay was carried out within 9 min. The retention times of amygdalin, mandelonitrile, prunasin, PTMT andbenzaldehyde were 3.14, 5.93, 6.82, 7.35 and 8.33 min, respectively. The mean absolute recoveries of three analysts were over 98%. The limit of detection and limit of quantification for were 0.02 and 0.04 μg/ml for amygdalin and benzaldehyde, 0.03 and 0.05 μg/ml for mandelonitrile, and 0.03 and 0.04 μg/ml for prunasin and PTMT.

scholarly journals Determination of the Contents of Antioxidants and Their Degradation Products in Sodium Chloride Injection for Blood Transfusion

2020 ◽  
Vol 2020 ◽  
pp. 1-12
Author(s):  
Bo Tao ◽  
Gang Wang ◽  
Zongning Yin ◽  
Xiaocong Pu ◽  
Yan Jiang ◽  
...  
Keyword(s):  
Sodium Chloride ◽  
Blood Transfusion ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Daily Intake ◽  
Gradient Elution ◽  
Hplc Method ◽  
Polymer Materials ◽  
Limit Of Quantification ◽  
Column Temperature

The infusion bag is mainly made up of polyolefin polymer. Antioxidants are usually added to these polymer materials in the production process to prevent the materials from aging and enhance the stability of the materials. Because of the potential harm of antioxidants to human body, it is necessary to limit the amount of antioxidants migrating to the pharmaceutical solutions. In the present study, we developed and validated the HPLC method for the simultaneous quantification of antioxidants and their degradation products migrating to sodium chloride solution for injection. A total of six antioxidants and six their degradation products were separated and simultaneously determined by using a Waters Symmetry RP18 column (250 × 4.6 mm, 5 μm) and gradient elution of methanol/acetonitrile/acetic acid-water (1 : 99, v/v) at a flow rate of 1.0 mL/min. The detective wavelength was set at 277 nm, and the column temperature was maintained at 35°C. The method was validated in terms of limit of detection (LOD, 0.011–0.151 μg/mL), limit of quantification (LOQ, 0.031–0.393 μg/mL), intraday precision (0.25%–3.17%), interday precision (0.47%–3.48%), linearity (0.1–46.8 μg/mL, r > 0.9994), stability (0.35%–3.29%), and accuracy (80.39%–104.31%). In the extraction experiment, antioxidants, BHT, 1010, 1330, 1076, and 168, and their degradation products, 1310 and DBP, were detected in the packaging materials. Only 1310 was detected in the migration experiment. The maximum daily dosage of sodium chloride for blood transfusion is three bags, and the content of 1310 in long-term testing samples is from 0 to 12 months ranging from 37.44 μg/3 bags to 48.71 μg/3 bags. The daily intake of 1310 did not exceed 48.71 μg, which was much lower than its permitted daily exposure (PDE, 300 μg/day). Therefore, the antioxidants and their degradation products migrating into the drug solution would not cause drug safety risks.

scholarly journals Reverse Phase Chiral HPLC Method for Enantiomeric Excess Determination of 2-Aminobutanamide

2019 ◽  
Vol 32 (1) ◽  
pp. 69-72
Author(s):  
T. Naga Jhansi ◽  
D. Pavan Kumar ◽  
Nagaraju Rajana ◽  
D. Jayadeep Kumar ◽  
G. Nageswara Rao
Keyword(s):  
Limit Of Detection ◽  
Enantiomeric Excess ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Perchloric Acid Solution ◽  
Column Temperature ◽  
Isomer Content

A reverse phase chiral HPLC method was developed for the determination of (R)-2-aminobutanamide isomer content in (S)-2-amino-butanamide key starting material for levetiracetam drug substance by using a CROWNPAK CR (+) column. Perchloric acid solution (0.05 %) was used as mobile phase and the flow rate was finalized as 0.3 mL/min. UV detection wavelength was 200 nm and column temperature was set as 15 ºC. The limit of detection and limit of quantification were 0.0002 mg/mL and 0.0005 mg/mL, respectively. The linearity calibration curve of (R)-2-aminobutanamide was shown good from the range of 0.0005 mg/mL to 0.004 mg/mL. The recovery of (R)-2-aminobutanamide isomer was between the range of 93 to 106 % in presence of (S)-2-aminobutanamide. The method was validated and found to be precise, accurate and robust. The method can be used for determination of (R)-2-aminobutanamide in presence of (S)-2-aminobutanamide, which is the key intermediate for preparation of levetiracetam. This method was validated in as per ICH Q2 (R1) and USP validation of compendial methods (1225).

scholarly journals Development and Validation of RP-Chiral HPLC Method for Determination of (R)-Enantiomer Excess Content in Efavirenz

2020 ◽  
Vol 32 (9) ◽  
pp. 2208-2212
Author(s):  
CH. RAMESH ◽  
DHARMASOTH RAMA DEVI DEVI ◽  
M.N.B. SRINIVAS ◽  
S. RADHA KRISHNA ◽  
NAGARAJU RAJANA ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Enantiomer Excess ◽  
Development And Validation ◽  
Methyl Phenyl

simple, specific, linear, accurate and precise reverse phase chiral HPLC method was developed for the separation of efavirenz enantiomers by using the Lux Amylose-2 column containing amylose tris(5-chloro-2-methyl phenyl carbamate) as a stationary phase. The mobile phase consists of 0.1 % formic acid in water and acetonitrile (55:45, v/v). The flow rate was kept at 1.0 mL/min and the detection wavelength used 252 nm and the column temperature was set at 25 ºC. The limit of detection was 0.01 mg/mL and the limit of quantification was 0.04 mg/mL. The linearity calibration curve of (R)-enantiomer was shown well from the range of 0.04 mg/mL to 0.4 mg/mL. The values of the correlation coefficient were 0.999 and 0.999 for (R)-enantiomer and (S)-efavirenz, respectively. The percentage recoveries of (R)-enantiomer from efavirenz drug substance were ranged from 93.5% to 107.5%. The results demonstrated that developed RP-chiral HPLC method was simple, precise, robust and applicable for the estimation of (R)-enantiomer in efavirenz API. This method was validated in as per ICH Q2 (R1) and USP validation of compendial methods <1225>.

scholarly journals Simple HPLC method for rapid quantification of nicotine content in e-cigarettes liquids

2020 ◽  
Author(s):  
Ala A. Alhusban ◽  
Samah A. Ata
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Negative Impact ◽  
Rapid Determination ◽  
Hplc Method ◽  
Correlation Factor ◽  
Photodiode Array Detection ◽  
Limit Of Quantification ◽  
Nicotine Content ◽  
Liquid Products

Abstract Electronic nicotine delivery systems (ENDs) are gaining popularity in Jordan as alternatives to tobacco cigarettes with an estimation of 10% of tobacco smokers switching to ENDs. Since nicotine is toxic and highly addictive substance, it is important to develop and validate an easy and rapid analytical method to accurately measure nicotine level in e-liquids. A simple high performance liquid chromatography–photodiode array detection (HPLC–PDA) method was developed and validated for rapid determination of the actual nicotine content in 11 of the most popular e-liquids brands available in the Jordanian market and compared to the nicotine levels appeared in the labeled packaging. The new method of analysis showed an excellent linearity with correlation factor equal to 0.9994 with analytical range between 100 and 1,000 µg/mL, and Limit of detection (LOD) and Limit of quantification (LOQ) of 32.6 µg/mL and 98.9 µg/mL, respectively. The results showed that the actual measured nicotine concentrations ranged from 0 to 25.81 mg/mL with percent deviation ranged from 63.1% less than to 3.24% more than the labeled concentration on packaging. And more than 10% deviation difference in actual nicotine concentrations versus labeled were found in 9 of the 11 e-liquid products (82%). In conclusion, nicotine labelling among e-liquids products have not accurately reflect the actual content which may have potential negative impact on users.

scholarly journals Development and Validation of New RP-HPLC Method for Simultaneous Determination of Methyl and Propyl Parabens with Levetiracetam in Pure Form and Pharmaceutical Formulation

2016 ◽  
Vol 2016 ◽  
pp. 1-5 ◽  
Author(s):  
Soad S. Abd El-Hay ◽  
Mostafa S. Mohram
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Gradient Elution ◽  
Hplc Method ◽  
Pure Form ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Limit Of Quantitation

A simple and robust high-performance liquid chromatography (HPLC) method is described for the assay for levetiracetam (LTC), methyl paraben (MHB), and propyl paraben (PHB) either in their pure form or in commercial Levepsy® syrup. The method is selective and stability indicating and all chromatographic conditions were studied to obtain adequate separation of LTC, MHB, and PHB from their degradation products and from excipients. The HPLC separation was carried out on a RP C18 Hypersil BDS analytical column (150 mm × 4.6 mm ID) using gradient elution system. The mobile phase flow rate was 1.5 mLmin−1 and the column temperature was kept at 40°C. Complete separation of the studied components was obtained within a cycle time of 8 min. LTC, MHB, and PHB were eluted at 1.56, 5.86, and 7.85 min, respectively. Detection was carried out at 240 nm using a dual wavelength detector. The method has been validated for linearity, accuracy, precision, specificity, limit of detection, limit of quantitation, robustness, and ruggedness. The proposed method was successfully applied for the determination of LTC in the presence of parabens in Levepsy syrup.

scholarly journals Development and Validation of a High-Performance Liquid Chromatography Method for Quality Assessment of Oriental Medicine, Dokhwalgisaeng-Tang

2021 ◽  
Vol 11 (17) ◽  
pp. 7829
Author(s):  
Chang-Seob Seo ◽  
Hyeun-Kyoo Shin
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Herbal Medicine ◽  
Formic Acid ◽  
Quality Assessment ◽  
High Performance ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Limit Of Quantification ◽  
Chromatography Method

Dokhwalgisaeng-tang (DHGST) is an herbal medicine formula that is frequently used in the treatment of arthritis in Korea and consists of 16 medicinal herbs. In this study, a simultaneous analysis method for quality assessment of DHGST by universal and widely used high-performance liquid chromatography was developed and validated. Twenty-four marker components were separated on a reverse-phase SunFire C18 column (4.6 × 250 mm, particle size; 5 μm) maintained at 40 °C using a gradient elution of two mobile phase systems (0.1% aqueous formic acid and 0.1% formic acid in acetonitrile). The developed method was validated via linearity, limit of detection, limit of quantification, recovery, and precision. Using the developed method, 24 marker components in DHGST were founded at 0.23–14.68 mg/g, and this method will be used as basic data for the quality assessment of DHGST or other herbal medicine prescriptions.

scholarly journals Developing and Validating a Method for Separating Flavonoid Isomers in Common Buckwheat Sprouts Using HPLC-PDA

Foods ◽  
2019 ◽  
Vol 8 (11) ◽  
pp. 549 ◽  
Author(s):  
Davin Jang ◽  
Young Sung Jung ◽  
Mi-Seon Kim ◽  
Seung Eel Oh ◽  
Tae Gyu Nam ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Common Buckwheat ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Mobile Phases ◽  
Germination Process ◽  
Relative Standard

Buckwheat sprouts that are synthesized during the germination process are rich in flavonoids, including orientin, vitexin, rutin, and their isomers (isoorientin, isovitexin, and quercetin-3-O-robinobioside, respectively). The purpose of this study was to optimize and validate an analytical method for separating flavonoid isomers in common buckwheat sprout extract (CSE). Factors, such as range, linearity, precision, accuracy, limit of detection, and limit of quantification, were evaluated for each standard using high-performance liquid chromatography (HPLC). On the basis of resolution and symmetry, a column temperature of 40 °C with 0.1% (v/v) acidic water and acetonitrile as mobile phases, at a flow rate of 1 mL min−1 were determined to be the optimal analytical conditions. Calibration curves for orientin, isoorientin, vitexin, isovitexin, and rutin exhibited good linearity with correlation coefficients of 0.9999 over the 6.25–100.00 μg mL−1 range. Recovery values of 96.67–103.60% confirmed that the method was accurate for all flavonoids. The relative standard deviations of intra-day repeatability and inter-day reproducibility confirmed method preciseness, with values of less than 5.21% and 5.40%, respectively. The developed method was used to analyze flavonoids in CSE, with isomers satisfactorily separated and simultaneously quantified. We demonstrated that the developed HPLC method can be used to monitor flavonoids in buckwheat sprouts.

scholarly journals A simple HPLC method containing greener modifier and slighter temperature elevated for simultaneous determination of three statin drugs in tablets

2021 ◽  
Author(s):  
Wael Alshitari ◽  
Fatimah Al-Shehri ◽  
Deia Abd El-Hady ◽  
Hassan M. Albishri
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Optimal Conditions ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Pharmaceutical Tablets ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Statin Drugs

AbstractStatins drugs are thought to be among the most prescribed drugs worldwide for the treatment of hypercholesterolaemia. A simple and reliable RP-HPLC method has been successfully employed for simultaneously separating and qualifying three statin drugs including atorvastatin, rosuvastatin and simvastatin in pharmaceutical tablets. The optimal conditions were mobile phase 50:50 (v/v) (formic acid pH 2.50: ETOH), column temperature 40.00 °C, detection wavelength 238.00 nm, and flow rate 1.00 mL/min. The proposed method has been validated based on the ICH guidelines in terms of linearity, precision, accuracy, and limit of detection and limit of quantification. The linear range investigated 2.0–80.0, 4.0–100.00, and 12.00–120.00 µg/mL for rosuvastatin, atorvastatin and simvastatin respectively with coefficients of determination (R2) within the range of 0.9993–0.9995. The LOD and LOQ for rosuvastatin, atorvastatin and simvastatin were (1.57, 4.76 µg/mL), (1.87, 5.66 µg/mL), (3.46, 10.49 µg/mL) respectively. In addition, in order to evaluate the feasibility of the method developed, it was employed towards the quantification of the pharmaceutical tablets for the analytes investigated and excellent recovery was obtained.

scholarly journals Determination of the Designer Drugs 3,4-Methylenedioxymethamphetamine, 3,4-Methylenedioxyethylamphetamine, and 3,4-Methylenedioxyamphetamine with HPLC and Fluorescence Detection in Whole Blood, Serum, Vitreous Humor, and Urine

2000 ◽  
Vol 46 (12) ◽  
pp. 1968-1977 ◽  
Author(s):  
Karine M Clauwaert ◽  
Jan F Van Bocxlaer ◽  
Els A De Letter ◽  
Serge Van Calenbergh ◽  
Willy E Lambert ◽  
...  
Keyword(s):  
Blood Serum ◽  
Whole Blood ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Vitreous Humor ◽  
Hplc Method ◽  
Designer Drugs ◽  
Fluorometric Detection ◽  
Limit Of Quantification

Abstract Background: The popular designer drugs 3,4-methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyethylamphetamine (MDEA) can be determined in serum, whole blood, and urine, but also in vitreous humor. The latter matrix is interesting when dealing with decomposed bodies in a toxicological setting. Methods: After extraction, chromatographic separation was achieved on a narrow-bore C18 column by gradient elution with fluorometric detection; results were confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Results: The method was linear over the range of 2–1000 μg/L for whole blood, serum, and vitreous humor, and 0.1–5 mg/L for urine. Extraction recoveries were &gt;70%, imprecision (CV) was 2.5–19%, and analytical recoveries were 95.5–104.4%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.8 and 2 μg/L, respectively, for whole blood, serum, and vitreous humor, and 2.5 μg/L and 0.1 mg/L, respectively, for urine. Excellent correlations between the quantitative LC-fluorescence and LC-MS/MS results were obtained. We found the following concentrations in a thanatochemical distribution study in rabbits: in serum, 5.3–685 μg/L for MDMA and from the LOQ to 14.5 μg/L for 3,4-methylenedioxyamphetamine (MDA); in whole blood, 19.7–710 μg/L for MDMA and from the LOQ to 17.8 μg/L for MDA; in vitreous humor, 12.1–97.8 μg/L for MDMA and from the LOQ to 3.86 μg/L for MDA. In routine toxicological urine samples, concentrations ranged from LOQ to 14.62 mg/L for MDA, from LOQ to 157 mg/L for MDMA, and from LOQ to 32.54 mg/L for MDEA. Conclusions: The HPLC method described is sensitive, specific, and suitable for the determination of MDMA, MDEA, and MDA in whole blood, serum, vitreous humor, and urine.

scholarly journals RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE COMBINATION OF IMIQUIMOD AND SALICYLIC ACID

2020 ◽  
pp. 41-48
Author(s):  
ANKITA SHARMA ◽  
INDER KUMAR ◽  
KARAN RANA
Keyword(s):  
Salicylic Acid ◽  
Method Development ◽  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Gradient Elution ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Rp Hplc

Objective: The present study was undertaken to develop and validate an RP-HPLC method for the combination of imiquimod and salicylic acid Methods: The method was carried out on Nucleodur C18 (250 mm × 4.6 mm I.D., 5 ????m) using low-pressure gradient elution mode. The mobile phase was used as 30M potassium dihydrogen phosphate and acetonitrile (45:55) pH 6.5 adjusted using ortho-phosphoric acid. The concentration of solvents was 1-20 µg/ml and the volume of injection was 20 mcl with the flow rate of 1.0 ml/min. The absorption maxima of salicylic acid and imiquimod were found 234 nm and 226 nm, respectively. Results: The method was validated and showed the linearity greater than 0.99% and with precision (RSD%<1). The limit of detection (LOD) and limit of quantification (LOQ) of salicylic acid was found to be 0.09756 µg/ml and 0.2956 µg/ml, respectively, and imiquimod was found to be 0.044031 µg/ml and 0.13334 µg/ml, respectively. Conclusion: The method developed in the present study was found to be sensitive, specific, and can be applied for the simultaneous estimation of imiquimod and salicylic acid.

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