hplc method
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2022 ◽  
Vol 69 (1) ◽  
pp. 17-29
Keiko Koizumi ◽  
Izumi Yoshida ◽  
Momochika Kumagai ◽  
Masahiro Ide ◽  
Tsuyoshi Kato ◽  

Molecules ◽  
2022 ◽  
Vol 27 (2) ◽  
pp. 543
Silvia Migliari ◽  
Antonino Sammartano ◽  
Marti Boss ◽  
Martin Gotthardt ◽  
Maura Scarlattei ◽  

Background: Glucagon-like peptide 1 receptor (GLP-1R) is preferentially expressed in pancreatic islets, especially in β-cells, and highly expressed in human insulinomas and gastrinomas. In recent years several GLP-1R–avid radioligands have been developed to image insulin-secreting tumors or to provide a tentative quantitative in vivo biomarker of pancreatic β-cell mass. Exendin-4, a 39-amino acid peptide with high binding affinity to GLP-1R, has been labeled with Ga-68 for imaging with positron emission tomography (PET). Preparation conditions may influence the quality and in vivo behavior of tracers. Starting from a published synthesis and quality controls (QCs) procedure, we have developed and validated a new rapid and simple UV-Radio-HPLC method to test the chemical and radiochemical purity of [68Ga]Ga-NODAGA-exendin-4, to be used in the clinical routine. Methods: Ga-68 was obtained from a 68Ge/68Ga Generator (GalliaPharma®) and purified using a cationic-exchange cartridge on an automated synthesis module (Scintomics GRP®). NODAGA-exendin-4 contained in the reactor (10 µg) was reconstituted with HEPES and ascorbic acid. The reaction mixture was incubated at 100 °C. The product was purified through HLB cartridge, diluted, and sterilized. To validate the proposed UV-Radio-HPLC method, a stepwise approach was used, as defined in the guidance document released by the International Conference on Harmonization of Technical Requirements of Pharmaceuticals for Human Use (ICH), adopted by the European Medicines Agency (CMP/ICH/381/95 2014). The assessed parameters are specificity, linearity, precision (repeatability), accuracy, and limit of quantification. Therefore, a range of concentrations of Ga-NODAGA-exendin-4, NODAGA-exendin-4 (5, 4, 3.125, 1.25, 1, and 0.75 μg/mL) and [68Ga]Ga-NODAGA-exendin-4 were analyzed. To validate the entire production process, three consecutive batches of [68Ga]Ga-NODAGA-exendin-4 were tested. Results: Excellent linearity was found between 5–0.75 μg/mL for both the analytes (NODAGA-exendin-4 and 68Ga-NODAGA-exendin-4), with a correlation coefficient (R2) for calibration curves equal to 0.999, average coefficients of variation (CV%) <2% (0.45% and 0.39%) and average per cent deviation value of bias from 100%, of 0.06% and 0.04%, respectively. The calibration curve for the determination of [68Ga]Ga-NODAGA-exendin-4 was linear with a R2 of 0.993 and CV% <2% (1.97%), in accordance to acceptance criteria. The intra-day and inter-day precision of our method was statistically confirmed using 10 μg of peptide. The mean radiochemical yield was 45 ± 2.4% in all the three validation batches of [68Ga]Ga-NODAGA-exendin-4. The radiochemical purity of [68Ga]Ga-NODAGA-exendin-4 was >95% (97.05%, 95.75% and 96.15%) in all the three batches. Conclusions: The developed UV-Radio-HPLC method to assess the radiochemical and chemical purity of [68Ga]Ga-NODAGA-exendin-4 is rapid, accurate and reproducible like its fully automated production. It allows the routine use of this PET tracer as a diagnostic tool for PET imaging of GLP-1R expression in vivo, ensuring patient safety.

2022 ◽  
Vol 20 (2) ◽  
pp. 383-387
Yahia Z. Tabaza ◽  
Kamal M. Mansi ◽  
Hanan A. Azzam ◽  
Farah F. Al-Mamoori ◽  
Ali M. Al-Samydai ◽  

Purpose: To develop a reversed phase high performance liquid chromatography (HPLC) method for the determination of dehydroepiandrosterone (DHEA) in dietary supplements. Methods: A reversed-phase high performance liquid chromatography (HPLC) method was developed for the determination of DHEA in dietary supplements. An isocratic system consisting of methanol and water (70:30 v/v) was run at a flow rate of 1 mL/min on a C18 HPLC column to achieve the separation. The method was validated with regard to linearity, intra-day and inter-day precision, and limits of both detection and quantification. Results: The method achieved a retention time of 10.8 min, a resolution of 4.12, a detection limit (LOD) of 50 ng/μL, a quantification limit (LOQ) of 166.7 ng/μL and a label claim of 108.6 % with a relative standard deviation (RSD) of 0.38 % over a range of 0.0625 – 0.50 mg/mL with a correlation coefficient of 0.9997. Conclusion: The method is simple, cost effective, time-saving and reliable for determining DHEA when compared to other reported methods in literature. Thus, it will be of benefit to manufacturers of this dietary supplement to adopt the method for quantitative laboratory analysis.

2022 ◽  
Vol 56 (1) ◽  
pp. 264-271
Mariadoss Alphonse ◽  
Rajasekaran Chandrasekaran ◽  
Michael Pillay ◽  
Devanand P Fulzele ◽  
Siva Ramamoorthy ◽  

2022 ◽  
Vol 56 (1) ◽  
pp. 32-42
Yik-Ling Chew ◽  
Hon-Kent Lee ◽  
Mei-Ann Khor ◽  
Kai-Bin Liew ◽  
Bontha Venkata Subrahmanya Lokesh ◽  

2022 ◽  
Vol 2022 ◽  
pp. 1-8
Wonjong Lee ◽  
Yoon-Bok Lee ◽  
Moon Haeng Huh ◽  
Jae Kwon Choi

Cyanocobalamin, which plays an essential role in the body, is a synthetic form used in medical food. This present study aimed to develop an HPLC analysis method for determination cyanocobalamin and investigate the stability of cyanocobalamin in medical food. Validation of the developed method for cyanocobalamin was evaluated with linearity, LOD, LOQ, and accuracy. The linearity of this method was calculated with a value of the coefficient of determination (R2) ≥ 0.999. LOD and LOQ were 0.165 and 0.499 μg/kg, respectively. The recovery of medical food matrixes for accuracy was more than 97.63%. The validated method was applied for determining cyanocobalamin from medical foods. The developed method was used to examine the additives for cyanocobalamin protection. Ferric chloride and sorbitol alleviated cyanocobalamin degradation from heat and ascorbic acid. Especially, sorbitol showed a superior protective effect during the medical food production process. Therefore, this study suggests that sorbitol is a sweetener additive that prevents cyanocobalamin degradation by heat and the food matrix in medical food processing.

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