Multi-Active Method (MAM) for the Analysis of Agriculture Product Technical Ingredients and Formulated Products

Toxicity of clomazone and its formulations to zebrafish embryos (Danio rerio)

Evaluation between ultrahigh pressure liquid chromatography and high-performance liquid chromatography analytical methods for characterizing natural dyestuffs

Suitable interface for coupling liquid chromatography to inductively coupled plasma-mass spectrometry for the analysis of organic matrices. 2 Comparison of Sample Introduction Systems

PT Bio Kusuma Pharmaceutical is a manufacturing company for pharmaceuticals, cosmetics and dietary supplements that was founded in 2003. The company is more engaged in topical medicines and creams for beauty. Increasing the existing market and productivity makes the company prioritize the success of production to increase the company's competitiveness. The increasing demand for products in the market has made PT Bio Kusuma Pharmaceutical have to increase its productivity. However, due to limited testing equipment in the laboratory, it is less effective in meeting the market. From August-October 2019, it showed a delay in testing due to too many batches of production but only one instrument in the laboratory. Production results that are not balanced with demand make the company unable to maximize its productivity due to inadequate testing equipment at the Quality Control laboratory. Based on data on comparison of production and testing in the laboratory where there is a delay in testing due to the inadequacy of the HPLC (High Performance Liquid Chromatography) testing instrument in the Quality Control (QC) laboratory, from this data the company requires additional HPLC (High Performance Liquid Chromatography) instrument tools. From the results of calculations using the AHP (Analytical Hierarchy Process) method, the HPLC (High Performance Liquid Chromatography) instrument from Acquity Arc (Waters) is obtained with a score of 0.46933 with evaluation factors for all criteria and 0.46932 with the ratio of benefits from alternatives.Keywords: Laboratory, HPLC (High Performance Liquid Chromatography), AHP (Analytical Hierarchy Process)

Delmopinol hydrochloride is widely used as an active ingredient (AI) in many human oral hygiene products. To the best of our knowledge (via literature search), there is no stability-indicating liquid chromatography method available in the public domain for assay and estimation of related substances of Delmopinol hydrochloride. A fast stability-indicating Reversed-Phase Ultra High-Performance Liquid Chromatography (RP-UHPLC) method has been developed and validated for identification, assay and estimation of related substances in commercial bulk batches of this AI. The major peak of the AI and its related compounds are adequately separated in 6min by a gradient elution on a hybrid silica-based C18 column (Waters Acquity UPLC® BEH C18, 50mm × 2.1mm I.D., 1.7μm particle size) maintained at 50°C. Mobile phase-A is composed of aqueous 10mM NH4OH and mobile phase-B is ACN. The AI and its related compounds are detected with UV detection at 220nm and quantitated by an external Delmopinol hydrochloride reference standard. The quantitation limit of the method is 0.1% of the target analytical concentration. This UHPLC method is fast and green and has been demonstrated to be specific, accurate, linear, precise, sensitive and robust as per ICH guidelines.

High performance liquid chromatography in pharmaceutical analyses

Ultra-high-pressure liquid chromatography (UHPLC) has emerged as the contemporary HPLC platform of choice in recent years. Because UHPLC requires less time for column equilibration and analysis, it is the perfect tool for developing methods quickly. The present state, advantages, and drawbacks of UHPLC in technique development are critically reviewed in this paper. To explain current developments and best practices, we employ case studies. Converting current HPLC methods to speedier analysis, quick screening of columns and mobile phases, and automated process optimisation are a few examples. Although the development of reversed-phase techniques for small-molecule pharmaceutical assay and impurity analysis is our primary emphasis, our findings and insights are applicable to other sample types and applications as well. When utilised with short, small-particle columns, UHPLC's greater pressure limitations not only produce quicker analysis but also make it possible to use longer columns more effectively for improved routine analysis of complicated materials.

Ultra-high-pressure liquid chromatography (UHPLC) in method development

Availability of Morphine Oral Solution for Childhood Cancer Patients in Low-Income Countries: Compounding and Stability Study in a Cote d'Ivoire University Teaching Hospital

Antibiotics are a therapy used in bacterial infections. The β-lactam group, such as penicillin, amoxicillin and cephalosporin are first generation antibiotics that can be used in treating bacterial infections. Antibiotics can be analyzed using High Performance Liquid Chromatography (HPLC). Ultra high performance liquid chromatography (UHPLC) and high pressure liquid chromatography (HPLC) are important analytical techniques in molecular separation. UHPLC is specifically designed for higher pressures during chromatographic analysis with short columns and small particle sizes, while HPLC aims to separate molecules in minimum time. Nonetheless, method transfer and revalidation between UHPLC and HPLC is quite easy and can save time. The use of these liquid chromatography techniques allows for more efficient and time-saving analysis. In performing routine HPLC analysis, it is important to consider speed, sensitivity, resolution, cost of analysis, and column maintenance. Therefore, modern developments in liquid chromatography are applied to save time and solvent consumption. Since 2004, UHPLC has repeatedly demonstrated significant advantages over HPLC-based methods. Parameters used in method data validation include precision, accuracy, coefficient of variation, limit of detection (LOD), and limit of quantity (LOQ).

The large chemical space occupied by natural products (NPs) is directly linked to a high variability of their intrinsic physicochemical properties that render their separation, detection and characterization challenging. The analysis of NPs in complex crude extracts requires efficient separation methods. In this respect, high-performance liquid chromatography (HPLC) has been recognized since the early 1980s as the most versatile technique for their profiling directly in crude mixtures without the need for complex sample preparation [1]. HPLC has greatly developed through the years in terms of convenience, speed, choice of column stationary phases, high sensitivity, applicability to a broad variety of sample matrices, and ability to hyphenate the chromatographic methods to spectroscopic detectors. The latest developments of HPLC, including the recent introduction of very pH-stable phases, sub-2-μm particles, monolith and fused core columns, have considerably improved the performances of HPLC. In particular in phytochemical analysis, the recent introduction of Ultra High Pressure Liquid Chromatography (UHPLC) systems operating at very high pressures and using sub-2 μm packing columns have allowed a remarkable decrease in analysis time and increase in peak capacity, sensitivity and reproducibility compared to conventional HPLC [2]. Such developments have a significant impact on the quality of data that can be obtained for metabolite profiling, dereplication studies and metabolomics when efficient spectroscopic detectors such as time–of-flight mass spectrometers (TOF)-MS are hyphenated to UHPLC. On the other hand, a good mastery of the chromatography parameters at the analytical scale enables efficient gradient transfer to the semi-preparative or the preparative scale based on chromatographic calculation. This efficient upscale allows high loading of crude mixture either for rapid at-line biological profiling of crude extracts with sensitive assay and/or de novo structure determination with microflow NMR methods with microgram of NPs. These developments, as well as other new trends in chromatography such as the renewed interest for superfluid critical fluid separation, the use of two dimensional LC or the hyphenation with additional separation efficiency in the gas phase provided by ion mobility in LC-MS hyphenation for the deconvolution of NPs in complex crude plant extracts will be discussed.

The large chemical space occupied by natural products (NPs) is directly linked to a high variability of their intrinsic physicochemical properties that render their separation, detection and characterization challenging. The analysis of NPs in complex crude extracts requires efficient separation methods. In this respect, high-performance liquid chromatography (HPLC) has been recognized since the early 1980s as the most versatile technique for their profiling directly in crude mixtures without the need for complex sample preparation.[1] HPLC has greatly developed through the years in terms of convenience, speed, choice of column stationary phases, high sensitivity, applicability to a broad variety of sample matrices, and ability to hyphenate the chromatographic methods to spectroscopic detectors. The latest developments of HPLC, including the recent introduction of very pH-stable phases, sub-2-µm particles, monolith and fused core columns, have considerably improved the performances of HPLC. In particular in phytochemical analysis, the recent introduction of Ultra High Pressure Liquid Chromatography (UHPLC) systems operating at very high pressures and using sub-2µm packing columns have allowed a remarkable decrease in analysis time and increase in peak capacity, sensitivity and reproducibility compared to conventional HPLC.[2] Such developments have a significant impact on the quality of data that can be obtained for metabolite profiling, dereplication studies and metabolomics when efficient spectroscopic detectors such as time-of-flight mass spectrometers (TOF)-MS are hyphenated to UHPLC. On the other hand, a good mastery of the chromatography parameters at the analytical scale enables efficient gradient transfer to the semi-preparative or the preparative scale based on chromatographic calculation. This efficient upscale allows high loading of crude mixture either for rapid at-line biological profiling of crude extracts with sensitive assay and/or de novo structure determination with microflow NMR methods with microgram of NPs. These developments, as well as other new trends in chromatography such as the renewed interest for superfluid critical fluid separation, the use of two dimensional LC or the hyphenation with additional separation efficiency in the gas phase provided by ion mobility in LC-MS hyphenation for the deconvolution of NPs in complex crude plant extracts will be discussed.

Extensive challenges faced by analytical chemists in studying real world complex samples such as biological body fluids, tissue samples, environmental and geological samples have led to the exponential growth in analytical techniques in the late twentieth century. This vast array of different analytical techniques can be categorized into two major areas: sample separation and mass spectrometry analysis. Current state-of-the-art sample separation methods include gas chromatography, high performance liquid chromatography, ultra high pressure liquid chromatography, solid phase extraction, capillary electrophoresis, capillary zone electrophoresis and gas phase separation techniques such as ion mobility spectrometry. The current trend in sample separation is to combine multiple techniques that utilize different separation mechanisms to maximize the separation. The most widely used combinations include two-dimensional gas chromatography, strong cation exchange or weak cation exchange chromatography followed by reversed-phase liquid chromatography, two-dimensional reversed-phase liquid chromatography, liquid chromatography followed by ion mobility spectrometry and two-dimensional electrophoresis techniques. The introduction of atmospheric pressure ionization techniques such as electrospray ionization and matrix assisted laser desorption ionization and the variations of these two techniques have exponentially increased the utility of mass spectrometry in complex sample analysis. Mass spectrometry itself has tremendously improved over the years in terms of sensitivity, detection limits and dynamic range capabilities. Currently, mass spectrometers can attain zeptomolar detection limits with five orders of magnitude dynamic range.

Two optimized and validated high performance liquid chromatography (HPLC) and spectrophotometric methods are proposed. The developed methods were quantified with high sensitivity, accuracy, and precision at low concentrations to determine rufinamide (RUF) in active pharmaceutical ingredients (API) and pharmaceutical preparations. HPLC method was developed using a base deactivated silica Hypersil C18 column and a combination of methanol: acetonitrile: water (15: 10: 75, v/v/v) as the mobile phase and detected at 210 nm. A reaction of RUF with sodium nitrite and hydrochloric acid occurred, absorbed maximally at 385 nm was extended to develop a ultraviolet (UV)-visible spectrophotometric method to determine RUF in API and pharmaceutical preparations. Different analytical validation parameters, including specificity, linearity, accuracy, precision, the limit of detection, quantification, ruggedness, and robustness, were determined as per International Conference on Harmonization guidelines. The linearity range of RUF was 0.15-3.5 and 10-100 μg/mL for HPLC and spectrophotometric methods, respectively. The proposed investigations were valuable for drug monitoring and regular analysis of RUF in quality control and research laboratories. Moreover, the accuracy and precision obtained with the UV-visible spectrophotometer implied that it could be a cheap, easy, and alternative method, while HPLC could be sensitive to determine RUF at low concentration levels.

Analytical validation is required as the basis for any evaluation activities during manufacturing process validation, cleaning validation and validation of the testing method itself in the pharmaceutical industry according to good manufacturing practice (GMP) rules and guidelines. Validation of analytical methods and procedures in a quality control (QC) laboratory is implemented mainly at the time of transfer or introduction of the methods developed by the analytical development laboratory within group companies or elsewhere. However, it is sometimes necessary to develop a new or improved method of analysis for the QC laboratory’s own use. In the first part of this report, a general description of analytical validation of the high performance liquid chromatography (HPLC) method including preparation of documents is presented based on the experience in our QC laboratory. A typical example of method validation of robotic analysis system is then cited. Finally the merits and demerits of these analytical validations for QC laboratories are summarized. The authors emphasize the importance of analytical validation and the responsibility of QC laboratory management for the effective design and implementation of validation activities.