Application of a HPLC-Q/TOF method with post-column compensation for separation and identification of polar impurities in Cytidine disodium triphosphate for injection

2021 ◽  
Vol 18 ◽  
Author(s):  
Jinqi Zheng ◽  
Mingjuan Zhao ◽  
Lishi Yang ◽  
Yue Chen ◽  
Xiao Gu ◽  
...  
Keyword(s):  
Ammonium Acetate ◽  
Degradation Products ◽  
Negative Ion ◽  
Acetate Solution ◽  
Nervous System Diseases ◽  
Isocratic Elution ◽  
Fragmentation Patterns ◽  
Negative Ion Mode ◽  
Cytidine Diphosphate ◽  
Aqueous Ammonium Acetate

Background: Cytidine Disodium Triphosphate (CTP-2Na) for injection is mainly used for treating nervous system diseases. Currently, there are few studies focused on the separation and identification of polar impurities in CTP-2Na for injection, which is important for ensuring drug safety and efficacy. Objective: The study aimed to establish an HPLC-Q/TOF method for the separation and identification of polar impurities in CTP-2Na for injection. Methods: Chromatographic separation was achieved on a Waters Atlantis T3 column using 5 mM aqueous ammonium acetate solution as the mobile phase in an isocratic elution mode. A postcolumn compensation technology was used to improve the ionization efficiency of impurities in the spray chamber. Results: Three polar impurities (disodium cytidine tetraphosphate, disodium cytidine diphosphate, disodium cytidine monophosphate) were detected in CTP-2Na for injection. The former one is probably the overreaction product during the production of CTP-2Na, the latter two were reported as degradation products. The fragmentation patterns of cytidine phosphate compounds in negative ion mode are summarized. Conclusion: This study provides a good reference for the separation and identification of polar impurities in nucleotide drugs.

scholarly journals Chromatography-tandem MASS spectrometry (HPLC-MS/MS) for the detection of valproic acid and its metabolites in blood plasma

2018 ◽  
Vol 10 (2) ◽  
pp. 35-42
Author(s):  
A. S. Malygin ◽  
N. S. Popov ◽  
M. A. Demidova ◽  
M. N. Kudrayshova
Keyword(s):  
Valproic Acid ◽  
Blood Plasma ◽  
Ammonium Acetate ◽  
Therapy Monitoring ◽  
Multiple Reaction Monitoring ◽  
Negative Ion ◽  
The Individual ◽  
Negative Ion Mode ◽  
Patients With Epilepsy ◽  
In Blood Plasma

Aim: to adapt the HPLC-MS/MS technique to determining valproic acid and its metabolites in blood plasma for drug therapy monitoring.Materials and Methods: The chromatographic assay was run using an Agilent 1260 Infinity II chromatograph with a Phenomenex synergi Fusion analytical column 4 μm-C18 2×50 mm. The mobile phase consisted of 0.1% ammonium acetate in distilled water and 0.1% ammonium acetate in methanol (10:90 v/v, 0.5 ml/min). The multiple ions monitoring (MIM) mode was used for mass- spectrometric detection of valproic acid at m/z = 143.1, with the negative ion mode. The method  was found applicable over the range from 1 mcg/ml to 200 mcg/ml of valproic acid. For the mass  spectroscopy detection of valproic acid metabolites, the multiple reaction monitoring (MRM mode)  was used. MS identifications of 2-propyl-4-pentanoil-β-О-glucuronide; 2-propyl-4-pentenoic acid,  3-hydroxy-2- propylpentanoic acid, 4-hydroxy-2-propylpentanoic acid, 2-propylglutaric acid and 3- oxo-2-propylpentanoic acid in the negative ion mode were carried out at m/z 319.2→143.2; m/z  140.1→140.1; m/z 159.1→101; m/z 159.1→123.1; m/z 173→129.1 and m/z 157.05→11,  respectively. The method was sensitive over the range from 10 ng/ml to 500 ng/ml of the tested  compounds.Results: The developed technique allows for determining valproic acid and its metabolites in a single sample; thus, the preliminary stage of separate sample preparation can be omitted, which increases the informative value of the assay without increasing its cost.Conclusion: This innovative methodology for the quantification of valproic acid and its metabolites in the blood plasma is expected to facilitate the individual approach to the treatment of patients with epilepsy, thereby increasing the efficacy and safety of the pharmacotherapy.

Characterization of Tear Gas Residues by Ion Mobility Spectrometry

1997 ◽  
Vol 51 (12) ◽  
pp. 1880-1889 ◽  
Author(s):  
Graeme Allinson ◽  
Cameron W. McLeod
Keyword(s):  
Ambient Temperature ◽  
Ion Mobility ◽  
Degradation Products ◽  
Negative Ion ◽  
Ion Mobility Spectrometer ◽  
Relative Standard ◽  
Acquisition Mode ◽  
Tear Gas ◽  
Negative Ion Mode

In this study a hand-held ion mobility spectrometer was used to characterize the vapors produced by α-chloroacetophenone (CN) and 2-chlorobenzylidenemalononitrile (CS), their isomers, and then-degradation products at ambient temperature and 50 °C, and in both the positive- and negative-ion acquisition modes. Minimum determinable residues were as follows: in the negative-ion acquisition mode at ambient temperature, CN 0.5 μg, CS 10 mg; at 50 °C, CN 0.5 μg, CS 16 μg; and in the positive-ion acquisition mode at ambient temperature, CN 0.5 μg, CS not detected; at 50 °C, CN 0.1 μg, CS not detected. The steady-state reproducibility was found to be independent of ion acquisition mode but dependent on signal intensity and background noise [relative standard deviation (RSD) 3–17%]—the smaller the signal, the greater the variation. The day-to-day variation in positive- and negative-mode signal intensities showed the same trends (RSD 3–33%). By comparing positive- and negative-ion mode spectra, it was possible to differentiate not only between CN and CS but also between their isomers and breakdown products.

scholarly journals Studies on structural elucidation of delphinium alkaloids by using LC-ESI-MS technique.

2015 ◽  
Vol 11 (3) ◽  
pp. 3399-3411
Author(s):  
Bilal Ahmad Dar ◽  
Mushtaq Ahmad Qurishi ◽  
Aijaz Hussain Kanth
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Negative Ion ◽  
Tentative Identification ◽  
Esi Ms ◽  
Short Run ◽  
Positive Mode ◽  
Fragmentation Patterns ◽  
Negative Ion Mode ◽  
Mode Response

A rapid,sensitive and specific liquid chromatography-electron spray-mass spectrometry (LC-ESI-MS) method to identify the different diester-diterpenoid and monoester type alkaloids from delphinium cashmerianum Collected from Sopi Kargil. Chromatographic separation were achieved on c-18 coloumn and peaks determined by mass spectrometry in positive and negative modes.The validated method led to tentative identification of eight alkaloids on the basis of their retention times and fragmentation patterns. Results showed that the positive mode response was much higher than the negative ion mode .chromatographic conditions were optimized to obtain high resolution and short run time.

scholarly journals Development and Validation of an HPLC/MS/MS Method for Determining the Thiazolidinone PG15 in Rat Plasma

2010 ◽  
Vol 93 (4) ◽  
pp. 1215-1221
Author(s):  
FláVia D T UchôA ◽  
Eduardo C Palma ◽  
Natalia F Souza ◽  
Maria C A Lima ◽  
Suely L Galdino ◽  
...  
Keyword(s):  
Internal Standard ◽  
Ammonium Hydroxide ◽  
Rat Plasma ◽  
Negative Ion ◽  
Pharmacokinetic Studies ◽  
Plasma Samples ◽  
Isocratic Elution ◽  
Negative Ion Mode ◽  
Development And Validation

Abstract A rapid, sensitive, and simple HPLC/MS/MS method was developed and validated for the determination of (5Z,E)-3-[2-(4-chlorophenyl)-2-oxoethyl]-5-(1H-indol-3-ylmethylene)-thiazolidine-2, 4-dione (PG15) in rat plasma using chlortalidone as an internal standard (IS). Analyses were performed using a C18 column and isocratic elution with acetonitrilewater (90 + 10, v/v) containing 10 mM ammonium hydroxide (pH 8.0) as the mobile phase pumped at 0.3 mL/min. Detection was performed by MS with negative ion mode electrospray ionization. Rat plasma samples were prepared by deproteinizing with acetonitrile. Detected fragments were 395.1 > 171.9 for PG15 and 337.3 > 189.9 for the IS. Calibration curves were linear from 10 to 1000 ng/mL, with the determination coefficient >0.99. The intraday and interday precisions were less than 12.2 and 11.3, respectively. The applicability of the HPLC/MS/MS method for pharmacokinetic studies was tested using plasma samples obtained after oral administration of PG15 to rats, and it provided the necessary sensitivity, linearity, precision, accuracy, and specificity.

A Stability-Indicating HPLC Method for the Quantification of Aliskiren and Hydrochlorothiazide in a Pharmaceutical Formulation

2014 ◽  
Vol 97 (6) ◽  
pp. 1519-1525 ◽  
Author(s):  
Dimitrios Karvelis ◽  
Eleni Kalogria ◽  
Irene Panderi
Keyword(s):  
Ammonium Acetate ◽  
Degradation Products ◽  
Hplc Method ◽  
Percentage Error ◽  
Forced Degradation ◽  
Content Uniformity ◽  
Isocratic Elution ◽  
Stability Indicating ◽  
Relative Percentage Error

Abstract A novel, fast, and sensitive stability-indicating HPLC method was developed, fully validated, and applied to the simultaneous determination of aliskiren and hydrochlorothiazide in a combined formulation. Effective chromatographic separation was achieved using a phenyl analytical column with isocratic elution using the mobile phase 0.030 M ammonium acetate–acetonitrile (60 + 40, v/v) at a flow rate of 0.40 mL/min. The UV spectrophotometric detector was set at 280 nm. The method was linear over the concentration ranges of 1.5–4.5 and 0.125–0.375 μg/mL for aliskiren and hydrochlorothiazide, respectively. The intraday and interday RSD values were less than 6.1%, while the relative percentage error, Er, was less than 5% for both analytes. Both drugs were subjected to stress conditions of acidic and alkaline hydrolysis, oxidation, and thermal degradation. The proposed method proved to be stability indicating by resolution of the drugs from their forced degradation products. The method was applied successfully to the QC and content uniformity tests in combined commercial tablets.

Confounding contaminants in mass spectrometric reaction monitoring

2018 ◽  
Author(s):  
Gilian T. Thomas ◽  
Landon MacGillivray ◽  
Natalie L. Dean ◽  
Rhonda L. Stoddard ◽  
Lars Yunker ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Mass Spectrometric ◽  
Negative Ion ◽  
Reaction Monitoring ◽  
Schlenk Flask ◽  
Dynamic Analyses ◽  
Rubber Septa ◽  
Negative Ion Mode ◽  
Mode A

<p>Reactions carried out in the presence of rubber septa run the risk of additives being leached out by the solvent. Normally, such species are present at low enough levels that they do not interfere with the reaction significantly. However, when studying reactions using sensitive methods such as mass spectrometry, the appearance of even trace amounts of material can confuse dynamic analyses of reactions. A wide variety of additives are present in rubber along with the polymer: antioxidants, dyes, detergent, and vulcanization agents, and these are all especially problematic in negative ion mode. A redesigned Schlenk flask for pressurized sample infusion (PSI) is presented as a means of practically eliminating the presence of contaminants during reaction analyses.</p>

scholarly journals Dopant-Enriched Nitrogen Gas for Enhanced Electrospray Ionization of Released Glycans in Negative Ion Mode

2021 ◽  
Author(s):  
Katarina Madunić ◽  
Sander Wagt ◽  
Tao Zhang ◽  
Manfred Wuhrer ◽  
Guinevere S.M. Lageveen-Kammeijer
Keyword(s):  
Electrospray Ionization ◽  
Negative Ion ◽  
Nitrogen Gas ◽  
Negative Ion Mode

Optimization of parameters affecting signal intensity in an LTQ-orbitrap in negative ion mode: A design of experiments approach

Talanta ◽  
2016 ◽  
Vol 147 ◽  
pp. 402-409 ◽  
Author(s):  
Nikolaos Lemonakis ◽  
Alexios-Leandros Skaltsounis ◽  
Anthony Tsarbopoulos ◽  
Evagelos Gikas
Keyword(s):  
Design Of Experiments ◽  
Signal Intensity ◽  
Negative Ion ◽  
Optimization Of Parameters ◽  
Negative Ion Mode ◽  
Mode A
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