Gas—liquid chromatographic determination of nitroglycerine in pharmaceutical preparations

Alley, Bernard J.; Dykes, Hiram W. H.

doi:10.1016/0021-9673(72)80021-9

Cited by 9 publications

(4 citation statements)

References 3 publications

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“…In order to assess contamination by submerged World War munitions as comprehensively as possible, with regard to present and future ecotoxicological consequences, the examination of large quantities of various abiotic and biotic samples for TNT, its metabolites, and other munitions components such as 1,3-dinitobenzene and 2,4-dinitrotoluene is required. Gas and liquid chromatography techniques have been routinely used in the detection of nitro-organic explosives for over fifty years [56,57]. Coupled to mass selective detectors, they do not only allow quantitative analysis, but also qualitative screening for unknown substances or unsuspected compounds in samples.…”

Section: A Toolbox For the Determination Of Nitroaromatic Explosives ...mentioning

confidence: 99%

Environmental and human toxicology studies on explosive chemicals leaking from submerged munitions

Maser,

Hartwig Bünning,

Strehse

2023

Propellants Explo Pyrotec

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This review provides an overview of 15 years of munitions research by the Institute of Toxicology and Pharmacology for Natural Scientists, University Medical School Schleswig‐Holstein, Kiel, Germany. As early as 2009, it was possible to detect the TNT metabolite 4‐ADNT in a quantity of 250 ng/g (wet weight) in blue mussels collected directly on munition items in the Kolberger Heide dumping area (Bight of Kiel, Baltic Sea, Germany). Based on these results, biomonitoring with blue mussels was established, in which uncontaminated mussels were exposed at certain distances from munition items and then retrieved after a few weeks in order to then be analyzed in the laboratory for energetic compounds (EC) including TNT and metabolites thereof. In following studies – in addition to mussels – also fish, sediments, water samples and passive samplers from specific locations were examined for the presence of EC. The study areas included dumping site regions from both the Baltic Sea and the North Sea, and were then extended to appropriate shipwrecks in the North Sea. The field studies were completed with laboratory investigations, which dealt with the development of a molecular biomarker as a kind of “early warning system” and with aspects of microbial degradation of EC. Finally, risk assessments for the marine environment and the human seafood consumer were carried out. The sections below are based on results from more than 10 scientific research projects and more than 20 publications in primary international research journals.

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Section: A Toolbox For the Determination Of Nitroaromatic Explosives ...mentioning

confidence: 99%

Environmental and human toxicology studies on explosive chemicals leaking from submerged munitions

Maser,

Hartwig Bünning,

Strehse

2023

Propellants Explo Pyrotec

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“…Alley and Dyes [53] used a gas chromatograph with a flame ionization detector. The analyses were performed at 130°C using a 60 cm´3 mm column filled with UCW-98 on Gas-Chrome Q at a helium flow rate of 40 ml/min.…”

Section: Quantitative Analysis Of Nitroglycerinmentioning

confidence: 99%

Nitroglycerin: Qualitative and quantitative analysis (A review)

2004

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Drugs containing nitrocompounds are frequently administered to patients suffering from cardiovascular disorders [1 -3]. In particular, nitroglycerin (I) is still widely used for the treatment of ischemic heart disease. This drug is available in various medicinal forms, including 0.0005 g tablets, 0.0005 and 0.001 g capsules (1% solution in oil), 1% ethanol solution, concentrated (1, 4, and 5 mg/ml) preparations for infusion, aerosols for sublingual administration (400 mg/dose), 2% ointment, and transdermal therapeutic systems.In the pure form, nitroglycerin (1,2,3-propanetrioltrinitrate) is a colorless oily liquid, which is also known as a dangerous explosive. Nitroglycerin is readily soluble in acetone, benzene, ether, methanol, acetic acid; it is also sparingly soluble in other alcohols, and poorly soluble in glycerol and water [4,5]. Being an ester, nitroglycerin possesses typical properties inherent in this class of compounds. At room temperature, nitroglycerin is stable in neutral media at pH 7.4, but decomposes in acid and alkaline media. At elevated temperatures, the rate of decomposition significantly increases [4 -6].Ready-to-use medicinal forms of nitroglycerin may contain impurities corresponding to the process of synthesis and the conditions of storage. The typical impurities are glycerin, nitrate and nitrite ions, di-and mononitroglycerins, ethylene glycol, diethylene glycol dinitrate, and others [7 -11].The broad range of possible concentrations of nitroglycerin and the possible presence of various impurities in the ready-to-use preparations necessitates the use of various methods for the analysis of these substances. The present review gives a summary of methods used for the analysis of nitroglycerin in the ready-to-use preparations currently available on the market. QUALITATIVE ANALYSIS OF NITROGLYCERINAccording to the State Pharmacopoeia (RSP-X) [12], nitroglycerin is identified using two qualitative reactions: alkaline hydrolysis (followed by the formation of acrolein) and a characteristic reaction for nitrates with diphenylamine.Foreign impurities in the ready-to-use preparations have to be determined by TLC and by paper chromatography. According to the pharmacopoeial articles for various particular ready-to-use preparations of nitroglycerin [9], foreign impurities are determined by TLC on Silufol or ATSKh plates with phosphor, which are eluted in toluene or a mixture of benzene, carbon tetrachloride, and dichloroethane (5 : 3 : 2). The spots are detected with the aid of a diphenylamine solution in chloroform and UV irradiation at 254 nm. Admitted impurities are diethylene glycol dinitrate, dinitroglycerin, and mononitroglycerin, at a total amount not exceeding 2%.It was also suggested to use TLC on silica gel plates eluted with tetrachloromethane, chloroform, ether, or the following mixtures: chloroform -ether (70 : 30) [13, 14]; chloroform -toluene (85 : 15) [7, 15]; tetrachloromethane -ether (1 : 1); tetrachloromethane -acetone (8 : 2), and tetrachloromethane -ethyl acetate (2 : 1) [16], ben...

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“…Gas and liquid chromatography techniques have been routinely used in the detection of nitro-organic explosives for over fifty years [9,10]. Coupled with mass selective detectors, they not only allow quantitative analysis but also qualitative screening for unknown substances or unsuspected compounds in samples.…”

Section: Introductionmentioning

confidence: 99%

A Toolbox for the Determination of Nitroaromatic Explosives in Marine Water, Sediment, and Biota Samples on Femtogram Levels by GC-MS/MS

Bünning¹,

Strehse²,

Hollmann³

et al. 2021

Toxics

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To determine the amount of the explosives 1,3-dinitrobenzene, 2,4-dinitrotoluene, 2,4,6-trinitrotoluene, and its metabolites in marine samples, a toolbox of methods was developed to enhance sample preparation and analysis of various types of marine samples, such as water, sediment, and different kinds of biota. To achieve this, established methods were adapted, improved, and combined. As a result, if explosive concentrations in sediment or mussel samples are greater than 10 ng per g, direct extraction allows for time-saving sample preparation; if concentrations are below 10 ng per g, techniques such as freeze-drying, ultrasonic, and solid-phase extraction can help to detect even picogram amounts. Two different GC-MS/MS methods were developed to enable the detection of these explosives in femtogram per microliter. With a splitless injector, limits of detection (LODs) between 77 and 333 fg/µL could be achieved in only 6.25 min. With the 5 µL programmable temperature vaporization—large volume method (PTV-LVI), LODs between 8 and 47 fg/µL could be achieved in less than 7 min. The detection limits achieved by these methods are among the lowest published to date. Their reliability has been tested and confirmed by measuring large and diverse sample sets.

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Gas—liquid chromatographic determination of nitroglycerine in pharmaceutical preparations

Cited by 9 publications

References 3 publications

Environmental and human toxicology studies on explosive chemicals leaking from submerged munitions

Environmental and human toxicology studies on explosive chemicals leaking from submerged munitions

Nitroglycerin: Qualitative and quantitative analysis (A review)

A Toolbox for the Determination of Nitroaromatic Explosives in Marine Water, Sediment, and Biota Samples on Femtogram Levels by GC-MS/MS

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