High Performance Liquid Chromatography (<scp>HPLC</scp>) in the Pharmaceutical Analysis

Levin, Shulamit

doi:10.1002/9780470571224.pse407

Cited by 12 publications

(7 citation statements)

References 124 publications

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“…25 The tailing factor was actually less for the lowest set of standards with a mean tailing factor of 1.1 ± 0.1. Statistical analysis of the tailing factors showed a significant difference in the tailing factors between the low concentration standards and the other two sets, but no difference existed between the two higher sets of standards as indicated by the statistical comparison summarized in Table 4.…”

Section: Resultsmentioning

confidence: 91%

“…Intra-day variation was calculated by determining the error of three sets of standards run within the day, and the inter-day variation was determined by running the standards for three consecutive days. 25 For the peak tailing factor, the USP method ( T = (a+b)/ 2a ) was utilized, where a = peak width from onset to midpoint at 5% peak height and b = peak width from midpoint to end at 5% of the peak height. 26 Statistical analysis was done using Sigmastat software (Systat Software, Inc., Chicago, IL).…”

Section: Methodsmentioning

confidence: 99%

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An ultra-high performance chromatographic method for the determination of artemisinin

Graves

Ledet

Nation

et al. 2014

Drug Development and Industrial Pharmacy

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Objective The goal of this study is to develop an ultra-high performance liquid chromatographic method for the quantitative determination of artemisinin at very low concentrations using selective ion mass spectroscopic detection. Materials and Methods Separation was conducted using a C4 100 mm × 2.1 mm column, and the mobile phase consisted of an isocratic two-component system consisting of 60% of a 0.1% aqueous solution of formic acid and 40% acetonitrile at a flow rate of 0.4 mL/min. The drug was detected by means of an electrospray mass spectrometer with selective ion monitoring of the [M-H2O+H]+ with m/z of 265.3 in positive ion mode. Results The calibration curves of artemisinin obtained from the UPLC/MS system were linear in the three ranges analyzed, with a correlation coefficient of no less than 0.9996 for all sets of standards. The peak tailing factor for all measurements were less than or equal to 1.7. The method proved to have good repeatability and linearity. Discussion The described analytical method reached a LOQ of 0.010 μg/mL with an isocratic system and enables an analysis rate of 20 samples per hour. The linearity of the standards was excellent for all sets of standards analyzed. Conclusion The method presented in this study provides a rapid and suitable means for the determination of artemisinin at very low concentrations. This is especially significant when performing dissolution studies where, due to the low solubility of artemisinin, a method that can measure the drug at nanogram levels is necessary.

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Section: Resultsmentioning

confidence: 91%

Section: Methodsmentioning

confidence: 99%

An ultra-high performance chromatographic method for the determination of artemisinin

Graves

Ledet

Nation

et al. 2014

Drug Development and Industrial Pharmacy

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“…Due to its simplicity and versatility, HPLC has become a cornerstone tool in pharmaceutical and biomedical analysis. HPLC is routinely used in drug discovery, development, and manufacturing, and routine assessment for the identification and quantification of drugs, both as active pharmaceutical ingredients and within their formulations [ 106 ]. In addition, it is essential for carrying out product characterizations, including assaying active pharmaceutical ingredients and profiling impurities [ 107 ], as well as degradation products generated by accelerated aging [ 108 ].…”

Section: Pharmaceutical Applicationsmentioning

confidence: 99%

“…In addition, it is essential for carrying out product characterizations, including assaying active pharmaceutical ingredients and profiling impurities [ 107 ], as well as degradation products generated by accelerated aging [ 108 ]. Moreover, the development of formulations requires studying dissolution properties, stability, and content uniformity of solid dosage forms, as well as conducting assays for the pharmaceutical formulations all of which are carried out using HPLC [ 106 , 109 ]. Although UV is the common detector for these applications, FLD was employed in several assays particularly in steroid analysis due to its sensitivity and selectivity as discussed below.…”

Section: Pharmaceutical Applicationsmentioning

confidence: 99%

High Performance Liquid Chromatography (HPLC) with Fluorescence Detection for Quantification of Steroids in Clinical, Pharmaceutical, and Environmental Samples: A Review

et al. 2022

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Steroids are compounds widely available in nature and synthesized for therapeutic and medical purposes. Although several analytical techniques are available for the quantification of steroids, their analysis is challenging due to their low levels and complex matrices of the samples. The efficiency and quick separation of the HPLC combined with the sensitivity, selectivity, simplicity, and cost-efficiency of fluorescence, make HPLC coupled to fluorescence detection (HPLC-FLD) an ideal tool for routine measurement and detection of steroids. In this review, we covered HPLC-FLD methods reported in the literature for the steroids quantification in clinical, pharmaceutical, and environmental applications, focusing on the various approaches of fluorescent derivatization. The aspects related to analytical methodology including sample preparation, derivatization reagents, and chromatographic conditions will be discussed.

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“…Radiochemical purity (RCP) is one of the most important quality criteria to release the final product for the clinical use, as described in the European Pharmacopeia [17][18][19]. To this aim, a validated separation method has to be available, enabling optimal separation between different (radio)chemical forms (radioactive impurities) other than the original intact radiopharmaceutical [27][28][29].…”

Section: Introductionmentioning

confidence: 99%

Development and Validation of an Analytical HPLC Method to Assess Chemical and Radiochemical Purity of [68Ga]Ga-NODAGA-Exendin-4 Produced by a Fully Automated Method

et al. 2022

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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.

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High Performance Liquid Chromatography (HPLC) in the Pharmaceutical Analysis

Cited by 12 publications

References 124 publications

An ultra-high performance chromatographic method for the determination of artemisinin

An ultra-high performance chromatographic method for the determination of artemisinin

High Performance Liquid Chromatography (HPLC) with Fluorescence Detection for Quantification of Steroids in Clinical, Pharmaceutical, and Environmental Samples: A Review

Development and Validation of an Analytical HPLC Method to Assess Chemical and Radiochemical Purity of [68Ga]Ga-NODAGA-Exendin-4 Produced by a Fully Automated Method

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