High-Performance Liquid Chromatographic Assay for Partially Nitrated Glycerins in Nitroglycerin

Baaske, David M.; Karnatz, Nancy N.; Carter, James E.

doi:10.1002/jps.2600720226

Cited by 9 publications

(3 citation statements)

References 15 publications

(16 reference statements)

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“…10 An internal standard was not necessary, since no extractions were involved in this analysis of NTG in parenteral fluids.…”

Section: Discussionmentioning

confidence: 99%

Nitroglycerin Adsorption to a Combination Polyvinyl Chloride, Polyethylene Intravenous Administration Set

Schaber¹,

Uden²,

McCoy³

1985

Drug Intelligence & Clinical Pharmacy

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Loss of nitroglycerin (NTG) from intravenous solutions to intravenous bags and administration sets has been well documented. This study was designed to examine a commercially available low adsorption administration set that was compatible with a volumetric infusion pump. A solution of NTG 100 micrograms/ml in dextrose 5% in glass bottles was used. Six study administration sets were tested. The infusion sets were connected to the NTG-containing glass bottles, filled as rapidly as possible, placed in the infusion pump, and set at the appropriate rate. Effluent was collected for NTG assay initially, and at 20 and 40 minutes, and 1, 1.5, 2, 3, 6, and 24 hours. The effects of flow rate were studied at 0.2 and 1.0 ml/min. The tubing performed similarly to other polyvinyl chloride (PVC)-containing sets at 0.2 ml/min and similar to non-PVC sets at 1.0 ml/min. The effect of an initial flush with 20-100 ml of 100 micrograms/ml NTG was also examined. An initial flush of 20 ml of 100 micrograms/ml NTG solution was found to enhance delivery of NTG immediately. NTG aliquots were stored frozen in glass vials prior to assay by high performance liquid chromatography.

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“…10 An internal standard was not necessary, since no extractions were involved in this analysis of NTG in parenteral fluids.…”

Section: Discussionmentioning

confidence: 99%

Nitroglycerin Adsorption to a Combination Polyvinyl Chloride, Polyethylene Intravenous Administration Set

Schaber¹,

Uden²,

McCoy³

1985

Drug Intelligence & Clinical Pharmacy

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“…Modified HPLC procedures were also described, which used alternative mobile phases such as acetonitrile -water (60 : 40) [58 -61], chloroform -hexane (60 : 40) [62], isooctane -ethanol [63], and isooctane -chloroform -methanol (80 : 13 : 7) [44]. Possible internal standards are isosorbide dinitrate [59], phthalimide solution [62], and anisole [60]. Titova et al used a standard sample prepared by triturating a 10% nitroglycerin solution with lactose.…”

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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“…Dimer species can also be formed from impurities in the starting sugar alcohol, such as the presence of diglycerol [9,10]. In addition to by-products formed during the reaction, a number of decomposition products, also partially nitrated species, may be created [4,6,7,9]. The relative amount of these impurities and degradation products are dependent on the route of synthesis and/or length of decomposition.…”

Section: Introductionmentioning

confidence: 99%

Direct analysis in real time mass spectrometry of potential by-products from homemade nitrate ester explosive synthesis

Sisco

Forbes

2016

Talanta

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This work demonstrates the coupling of direct analysis in real time (DART) ionization with time-of-flight mass spectrometry (MS) in an off-axis configuration for the trace detection and analysis of potential partially nitrated and dimerized by-products of homemade nitrate ester explosive synthesis. Five compounds relating to the synthesis of nitroglycerin (NG) and pentaerythritol tetranitrate (PETN) were examined. Deprotonated ions and adducts with molecular oxygen, nitrite, and nitrate were observed in the mass spectral responses of these compounds. A global optimum temperature of 350 °C for the by-products investigated here, enabled single nanogram to sub nanogram trace detection. Matrix effects were examined through a series of mixtures containing one or more compounds (sugar alcohol precursors, by-products, and/or explosives) across a range of mass loadings. The explosives MS responses experienced competitive ionization in the presence of all by-products. The magnitude of this influence corresponded to both the degree of by-product nitration and the relative mass loading of the by-product to the explosive. This work provides a characterization of potential by-products from homemade nitrate ester synthesis, including matrix effects and potential challenges that might arise from the trace detection of homemade explosives (HMEs) containing impurities. Detection and understanding of HME impurities and complex mixtures may provide valuable information for the screening and sourcing of homemade nitrate ester explosives.

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High-Performance Liquid Chromatographic Assay for Partially Nitrated Glycerins in Nitroglycerin

Cited by 9 publications

References 15 publications

Nitroglycerin Adsorption to a Combination Polyvinyl Chloride, Polyethylene Intravenous Administration Set

Nitroglycerin Adsorption to a Combination Polyvinyl Chloride, Polyethylene Intravenous Administration Set

Nitroglycerin: Qualitative and quantitative analysis (A review)

Direct analysis in real time mass spectrometry of potential by-products from homemade nitrate ester explosive synthesis

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