Methods for simultaneous determination of 29 legacy and insensitive munition (IM) constituents in aqueous, soil-sediment, and tissue matrices by high-performance liquid chromatography (HPLC)

2021 ◽  
Author(s):  
Bobbi Stromer ◽  
Rebecca Crouch ◽  
Katrinka Wayne ◽  
Ashley Kimble ◽  
Jared Smith ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Solvent Extraction ◽  
Environmental Protection Agency ◽  
High Performance ◽  
Solid Phase ◽  
Degradation Products ◽  
Direct Injection ◽  
High Water ◽  
Hplc Method

Standard methods are in place for analysis of 17 legacy munitions compounds and one surrogate in water and soil matrices; however, several insensitive munition (IM) and degradation products are not part of these analytical procedures. This lack could lead to inaccurate determinations of munitions in environmental samples by either not measuring for IM compounds or using methods not designed for IM and other legacy compounds. This work seeks to continue expanding the list of target analytes currently included in the US Environmental Protection Agency (EPA) Method 8330B. This technical report presents three methods capable of detecting 29 legacy, IM, and degradation products in a single High Performance Liquid Chromatography (HPLC) method with either ultraviolet (UV)-visible absorbance detection or mass spectrometric detection. Procedures were developed from previously published works and include the addition of hexahydro-1-nitroso-3,5-dinitro-1,3,5-triazine (MNX); hexahydro-1,3-dinitroso-5-nitro-1,3,5-triazine (DNX); hexahydro-1,3,5-trinitroso-1,3,5-triazine (TNX); 2,4-diamino-6-nitrotoluene (2,4-DANT); and 2,6-diamino-4-nitrotoluene (2,6-DANT). One primary analytical method and two secondary (confirmation) methods were developed capable of detecting 29 analytes and two surrogates. Methods for high water concentrations (direct injection), low-level water concentrations (solid phase extraction), soil (solvent extraction), and tissue (solvent extraction) were tested for analyte recovery of the new compounds.

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 A NEW HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SEPARATION AND SIMULTANEOUS QUANTIFICATION OF EPTIFIBATIDE AND ITS IMPURITIES IN PHARMACEUTICAL INJECTION FORMULATION

2021 ◽  
pp. 165-172
Author(s):  
K. SRI GIRIJA ◽  
BIKSHAL BABU KASIMALA ◽  
VENKATESWARA RAO ANNA
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Ultra Violet ◽  
Hplc Method ◽  
Chromatography Method ◽  
Standard Drug ◽  
Pharmaceutical Dosage Forms ◽  
Relative Standard

Objective: The objective of the present study is to develop a stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for qualitative and quantitative determination of Eptifibatide and its impurities in bulk and pharmaceutical dosage forms. Methods: The chromatographic separation was carried on Phenomenex Luna C18 column (250 mm×4.6 mm; 5µ id) as stationary phase, methanol and phosphate buffer at pH 6.4 in the ratio of 65:45 (v/v) as mobile phase at flow rate of 1.0 ml/min, Ultra Violet (UV) detection was carried at the wavelength of 236 nm and the analysis was completed with a run time of 15 min. Results: In the developed conditions, the retention time of Eptifibatide and its impurities 1 and 2 were found to be 3.35, 4.93 and 8.18 min, respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability and robustness. Spiked recovery at 50%, 100% and 150% was carried for both standard and impurities and the acceptable % recovery of 98-102 was observed for Eptifibatide and both impurities studied and the % Relative standard deviation (RSD) in each spiked level was found to be less than 2. Stability tests were done through the exposure of the analyte solution to five different stress conditions i. e expose to 1N Hydrochloric acid (HCl), 1 N Sodium hydroxide (NaOH), 3% Hydrogen peroxide (H2O2), 80 °C temperature to UV radiation. In all the degradation conditions, standard drug Eptifibatide was detected along with both the impurities studied and the degradation products were successfully separated. In the formulation analysis, there is no other chromatographic detection of other impurities and formulation excipients. Conclusion: The developed method was found to be suitable for the quantification of Eptifibatide and can separate and analyse impurities 1 and 2.

Development and Validation of a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) Method for Identification, Assay and Estimation of Related Substances of Ivermectin in Bulk Drug Batches of Ivermectin Drug Substance

2021 ◽  
Author(s):  
Daoli Zhao ◽  
Rasangi M Wimalasinghe ◽  
Lin Wang ◽  
Abu M Rustum
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Drug Substance ◽  
Related Impurities ◽  
Rp Hplc ◽  
Bulk Drug

Abstract A reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed and validated for the identification and assay of Ivermectin, including the identification and estimation of its process-related impurities and degradation products in bulk drug substance of Ivermectin. Analytes were separated on a HALO C18 column (100 mm × 4.6 mm I.D., 2.7 μm particle size) maintained at 40 °C (column temperature) with gradient elution. All analytes of interests were adequately separated within 25 min. All degradation products, process-related impurities and assay were monitored by ultraviolet detection at 254 nm. The new HPLC method described here successfully separated an isomer peak of the active pharmaceutical ingredient (API) from the major API peak. This newly separated isomer peak is around 1.2 to 1.5% (peak area) in typical API samples, and coelutes with the major API peak by all current HPLC methods. Quantitation limit of the HPLC method is 0.1% of target analytical concentration (~1.0 μg/mL). This method has been demonstrated to be accurate, robust, significantly higher degree of selectivity compared to the HPLC methods of Ivermectin drug substance reported in the literature and in the compendial HPLC methods prescribed in the current USA and European Pharmacopeia.

scholarly journals Solid Phase Micro Tip Extraction Coupled With High Performance Liquid Chromatography for Diclofenac Sodium Analysis in Urine Sample

2013 ◽  
Vol 9 (1) ◽  
Author(s):  
Dadan Hermawan ◽  
Law Hui Ling ◽  
Wan Aini Wan Ibrahim ◽  
Mohd Marsin Sanagi
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Urine Sample ◽  
High Performance ◽  
Solid Phase ◽  
Diclofenac Sodium ◽  
Hplc Method ◽  
Urine Samples ◽  
Preparation Technique ◽  
Mobile Phase Flow Rate

A solid phase micro tip extraction (SPMTE) has been developed as sample preparation technique for the analysis of diclofenac sodium, a non-steroidal anti-inflammatory drug (NSAID) in human urine sample. The analysis was performed by high performance liquid chromatography (HPLC) system using methanol:water (60:40, v/v) as mobile phase, flow rate of 1.0 mL/min under UV detection wavelength at 282 nm. Extraction conditions such as desorption solvent and extraction time were optimized in this study. The optimized SPMTE coupled with the HPLC method was successfully applied for the determination of diclofenac sodium in urine samples. The best recovery of diclofenac sodium in urine samples is 74.80% with RSD of 3.56% (n=3). The proposed method provides simple and rapid analysis of diclofenac sodium in urine sample.

scholarly journals DETERMINATION OF FORMALDEHYDE IN WATER BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY WITH THE USE OF SOLID PHASE EXTRACTION

2019 ◽  
Vol 96 (3) ◽  
pp. 281-284 ◽  
Author(s):  
P. P. Kochetkov ◽  
A. G. Malysheva ◽  
V. V. Glebov
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
High Performance ◽  
Solid Phase ◽  
Hplc Method ◽  
Phase Extraction ◽  
Definition Of ◽  
Quantitative Definition

The way of definition of formaldehyde in water by the method of high performance liquid chromatography (HPLC) with the use of solid-phase extraction for concoction and extraction of the analyzed derivative formaldehyde is presented. The method is distinguished by the simplified and accelerated procedure of the sample preparation in comparison with classical liquid extraction. Chromatographic division of substances was reached on the turned phase column C18 with the use of mixture of the deionized water and an acetonitrile as a mobile phase. Definition was carried out at absorption wavelength of 360 nanometers. Linearity was reached in the ranges of concentration from 1 to 200 mcg/l. Full validation of a method is carried out. For control samples of all levels, including the lower limit of quantitative definition, the value of repeatability (RSD) accounted for ≤15%. The index of the accuracy amounted to ≤10%. The presented way showed good validation characteristics and can be recommended for the simplification and acceleration of the determination of the content of formaldehyde in water by the HPLC method

scholarly journals Determination of Biotin by High-Performance Liquid Chromatography in Infant Formula, Medical Nutritional Products, and Vitamin Premixes

2006 ◽  
Vol 89 (6) ◽  
pp. 1515-1518 ◽  
Author(s):  
Linda B Thompson ◽  
Daniel J Schmitz ◽  
Shang-Jing Pan
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Infant Formula ◽  
High Performance ◽  
Solid Phase ◽  
Reversed Phase ◽  
Hplc Method ◽  
Fluorescence Detector ◽  
Sample Preparation Procedure

Abstract A solid-phase extraction sample preparation procedure was developed for use with a high-performance liquid chromatography (HPLC) method for biotin analysis. The HPLC method used a reversed-phase C18 column; chromatography run time was 8.5 min. After eluting from the column, biotin went through postcolumn reaction to form a conjugate with streptavidinfluorescein isothiocyanate, which was then detected by a fluorescence detector. This method was tested with infant formula, medical nutritional products, and vitamin premix samples.

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