scholarly journals Development and Validation of a GMP-Compliant High-Pressure Liquid Chromatography Method for the Determination of the Chemical and Radiochemical Purity of [18F]PSMA-1007, a PET Tracer for the Imaging of Prostate Cancer

2021 ◽  
Vol 14 (3) ◽  
pp. 188
Author(s):  
Ines Katzschmann ◽  
Heike Marx ◽  
Klaus Kopka ◽  
Ute Hennrich
Keyword(s):  
Prostate Cancer ◽  
Quality Control ◽  
Radiochemical Purity ◽  
Control Method ◽  
Solid Phase ◽  
Hplc Method ◽  
Attractive Alternative ◽  
Chromatography Method ◽  
Pet Tracer

For the PET imaging of prostate cancer, radiotracers targeting the prostate-specific membrane antigen (PSMA) are nowadays used in clinical practice. [18F]PSMA-1007, a radiopharmaceutical labeled with fluorine-18, has excellent properties for the detection of prostate cancer. Essential for the human use of a radiotracer is its production and quality control under GMP-compliance. For this purpose, all analytical methods have to be validated. [18F]PSMA-1007 is easily radiosynthesized in a one-step procedure and isolated using solid phase extraction (SPE) cartridges followed by formulation of a buffered injection solution and for the determination of its chemical and radiochemical purity a robust, fast and reliable quality control method using radio-HPLC is necessary. After development and optimizations overcoming problems in reproducibility, the here described radio-HPLC method fulfills all acceptance criteria—for e.g., specificity, linearity, and accuracy—and is therefore well suited for the routine quality control of [18F]PSMA-1007 before release of the radiopharmaceutical. Recently a European Pharmacopeia monograph for [18F]PSMA-1007 was published suggesting a different radio-HPLC method for the determination of its chemical and radiochemical purity. Since the here described method has certain advantages, not least of all easier technical implementation, it can be an attractive alternative to the monograph method. The here described method was successfully validated on several radio-HPLC systems in our lab and used for the analysis of more than 60 batches of [18F]PSMA-1007. Using this method, the chemical and radiochemical purity of [18F]PSMA-1007 can routinely be evaluated assuring patient safety.

scholarly journals A validated high performance liquid chromatography method for determination of three bioactive compounds p-hydroxy benzoic acid, negundoside and agnuside in Vitex species

2015 ◽  
Vol 34 (2) ◽  
pp. 321 ◽  
Author(s):  
Tushar Dhanani ◽  
Sonal Shah ◽  
Satyanshu Kumar
Keyword(s):  
Benzoic Acid ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Hplc Method ◽  
Vitex Negundo ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Vitex Species

A validated rapid and simple isocratic HPLC-PDA method was developed for identification and quantification of p- hydroxy benzoic acid and two iridoids negundoside and agnuside in the extracts of two Vitex species, Vitex negundo and Vitex trifolia. The separation of the three compounds was achieved on a RP-18 (250 mm X 4 mm, 5µm) column at 25o C using acetonitrile (15%) and 0.05% trifluoroacetic acid (TFA) in water (85%). Limit of detection (LOD) were 1, 2.5 and 2.5 μg/ml for p- hydroxy benzoic acid, negundoside and agnuside respectively. Similarly, limit of quantification (LOQ) were 2.5, 5 and 5 μg/ml for p- hydroxy benzoic acid, negundoside and agnuside respectively. Good linearity (r2 > 0.999) was observed for all the three compounds in wide concentration range. Using the developed HPLC method, the three compounds were identified and quantified in leaves and bark extracts of Vitex negundo and Vitex trifolia. The novelty of the developed HPLC method is that it does not require complex sample processing such as use of solid phase extraction as well as use of buffer in mobile phase. This is the first report of a validated HPLC method for the simultaneous determination of p- hydroxy benzoic acid, negundoside and agnuside in Vitex species.

scholarly journals A Validated LC Method for Separation and Determination of Tetralone-4-O-β-D-Glucopyranoside and 4-Hydroxy-α-Tetralone in Ammannia multiflora

2012 ◽  
Vol 2012 ◽  
pp. 1-4 ◽  
Author(s):  
Harish C. Upadhyay ◽  
Ram K. Verma ◽  
Santosh K. Srivastava
Keyword(s):  
Quality Control ◽  
Flow Rate ◽  
Control Method ◽  
Hplc Method ◽  
Assay Method ◽  
Good Linearity ◽  
Rp Hplc ◽  
Quality Control Method ◽  
Calibration Curves

A rapid, sensitive, and reproducible RP-HPLC method was developed for the determination of two constituents in Ammannia multiflora, namely, tetralone-4-O-β-D-glucopyranoside (1) and 4-hydroxy-α-tetralone (2). The samples were separated on a Spherisorb ODS2 column (250×4.6 mm, i.d., 10 μm) and binary elution of water and methanol (2 : 3) with flow rate of 0.8 mL/min at λ 254 nm. The LOD and LOQ were found 0.05 and 0.18 μg/mL for compound 1 and 0.06 and 0.18 μg/mL for compound 2, respectively. All calibration curves showed good linearity (r2>0.999) within test ranges for both the analytes. The RSD values for intra-and inter-day precisions were less than 1.1%. The successful application of the developed method on five different samples revealed an average 0.0206% and 0.7636% (w/w) of compounds 1 and 2, respectively in A. multiflora indicating that the developed LC assay method may be readily utilized as a quality control method for the plant.

Determination of Radiochemical Purity and Pharmacokinetic Parameters of 99mTc-Sulphur Colloid and 99mTc-Tin Colloid

1981 ◽  
Vol 20 (06) ◽  
pp. 279-282 ◽  
Author(s):  
D. Konstantinovska ◽  
K. Milivojević ◽  
J. Bzenić ◽  
V. Jovanović
Keyword(s):  
Radiochemical Purity ◽  
Slow Component ◽  
Pharmacokinetic Parameters ◽  
Optimum Size ◽  
Buffer Solution ◽  
Chromatography Method ◽  
Fast Phase ◽  
Biodistribution Studies ◽  
Biological Half Time

Labelling yield and radiochemical purity, higher than 95%, of 99mTc-colloid preparations were determined by using the paper chromatography method. Less than 3% of labelled citric acid, added to the preparation as a buffer solution, has been found in 99mTc-sulphur colloid. High radiochemical purity and optimum size of colloid particles has also been proved by biodistribution studies on experimental animals. The analysis performed has shown that more than 50% of 99mTc-colloid preparations excreted by urine is 99mTcO–, the remaining past 50% being protein bound 99mTc. Biological half-time of excretion of the fast phase is the same for both preparations, i.e. 10 min, while for the slow component it is 120 min in 99mTc-S-colloid and 160 min in 99mTc-Sn colloid.

Developing a High-performance Liquid Chromatography Method for Simultaneous Determination of Loratadine and its Metabolite Desloratadine in Human Plasma

2020 ◽  
Vol 20 (13) ◽  
pp. 1053-1059
Author(s):  
Mahmoud M. Sebaiy ◽  
Noha I. Ziedan
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Allergic Diseases ◽  
Reversed Phase ◽  
Hplc Method ◽  
H1 Receptor ◽  
Chromatography Method

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.

Chemical Fingerprint Analysis and Simultaneous Determination of Nucleosides and Amino Acids in Kang Fu Xin Liquid by High Performance Liquid Chromatography with Diode Array Detector

2020 ◽  
Vol 16 (7) ◽  
pp. 831-843
Author(s):  
Yuwen Wang ◽  
Shuping Li ◽  
Liuhong Zhang ◽  
Shenglan Qi ◽  
Huida Guan ◽  
...  
Keyword(s):  
Amino Acids ◽  
Quality Control ◽  
Uric Acid ◽  
Control Method ◽  
Principal Component ◽  
Gradient Elution ◽  
Hplc Method ◽  
Array Detector ◽  
Fingerprint Analysis ◽  
Wavelength Switching

Background and Objective: Kang Fu Xin liquid (KFX) is an official preparation made from the ethanol extract product from P. Americana. The present quality control method cannot control the quality of the preparation well. The aim of the present study is to establish a convenient HPLC method for multicomponents determination combined with fingerprint analysis for quality control of KFX. Methods: An HPLC-DAD method with gradient elution and detective wavelength switching program was developed to establish HPLC fingerprints of KFX, and 38 batches of KFX were compared and evaluated by similarity analysis (SA), hierarchical clustering analysis (HCA), and principal component analysis (PCA). Meanwhile, six nucleosides and three amino acids, including uracil, hypoxanthine, uric acid, adenosine, xanthine, inosine, tyrosine, phenylalanine and tryptophan in KFX were determined based on the HPLC fingerprints. Results: An HPLC method assisted with gradient elution and wavelength switching program was established and validated for multicomponents determination combined with fingerprint analysis of KFX. The results demonstrated that the similarity values of the KFX samples were more than 0.845. PCA indicated that peaks 4 (hypoxanthine), 7 (xanthine), 9 (tyrosine), 11, 13 and 17 might be the characteristic contributed components. The nine constituents in KFX, uracil, hypoxanthine, uric acid, adenosine, xanthine, inosine, tyrosine, phenylalanine and tryptophan, showed good regression (R2 > 0.9997) within test ranges and the recoveries of the method for all analytes were in the range from 96.74 to 104.24%. The limits of detections and quantifications for nine constituents in DAD were less than 0.22 and 0.43 μg•mL-1, respectively. Conclusion: The qualitative analysis of chemical fingerprints and the quantitative analysis of multiple indicators provide a powerful and rational way to control the KFX quality for pharmaceutical companies.

scholarly journals A Selective High-Performance Liquid Chromatography Method for the Determination of Reboxetine in Bulk Drug and Tablets

2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Depressive Disorders ◽  
Degradation Products ◽  
Severe Depression ◽  
Hplc Method ◽  
Chromatography Method ◽  
Relative Standard

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.

scholarly journals Development and validation of a bioanalytical LC-UV method with solid-phase extraction for determination of valproic acid in saliva

2012 ◽  
Vol 62 (2) ◽  
pp. 211-220 ◽  
Author(s):  
Jasmina Tonic-Ribarska ◽  
Arlinda Haxhiu ◽  
Zoran Sterjev ◽  
Gordana Kiteva ◽  
Ljubica Suturkova ◽  
...  
Keyword(s):  
Valproic Acid ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Human Saliva ◽  
Hplc Method ◽  
Therapeutic Monitoring ◽  
Phase Extraction ◽  
Free Drug Concentration ◽  
Development And Validation

Development and validation of a bioanalytical LC-UV method with solid-phase extraction for determination of valproic acid in saliva A bioanalytical HPLC method with UV detection for the determination of the antiepileptic drug valproic acid in human saliva has been developed and validated. Saliva represents an alternative matrix for therapeutic monitoring of antiepileptic drugs due to the increasing interest in free drug concentration. The proposed method involved solid-phase extraction for sample preparation and yielded very good mean recoveries of 99.4 % and 97.9 % for valproic acid and IS, respectively. The calibration function for valproic acid was linear over the concentration range of 1.0-50.0 μg mL-1 (R2 = 0.9989). Within-run and between-run precision and accuracy were studied at four concentrations and RSDs were less than 7.3 and 2.2 %, while accuracy values were higher than 96.8 and 97.5 %, respectively. The described method provides sensitivity, linearity, precision, accuracy and is suitable for analyses of valproic acid in saliva samples.

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