A Selective and Sensitive Method Development and Validation of 1,1-Dimethyl-3-Hydroxy-Pyrrolidinium Bromide Impurity in Glycopyrrolate Oral Solution by Liquid Chromatography–Tandem Mass Spectroscopy

2021 ◽  
Author(s):  
Rajesh Kumar Chawla ◽  
G S N Koteswara Rao ◽  
Umasankar Kulandaivelu ◽  
Siva Prasad Panda ◽  
Rajasekhar Reddy Alavala
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Method Development ◽  
Limit Of Detection ◽  
Oral Solution ◽  
Calibration Plot ◽  
Tandem Mass ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Abstract Objective A selective and sensitive liquid chromatography–tandem mass spectrometer (LC–MS/MS) method has been developed for the quantification of 1,1-dimethyl-3-hydroxy-pyrrolidinium bromide impurity in glycopyrrolate oral solution. Materials and method The LC–MS/MS analysis was done on X Bridge HILIC (100 × 4.6 mm, 5 μm) analytical column, and the mobile phase used was10 mM ammonium formate with 0.2% formic acid as mobile phase-A and acetonitrile as mobile phase-B with a gradient programme of 5.0 min. The flow rate used was 1.2 mL/min. Triple quadrupole mass detector coupled to positive electrospray ionization operated in multiple reactions monitoring mode was used for the quantification at m/z 116.10 ± 0.5. Results Retention time of impurity was found ~3.2 min. The method was validated in terms of specificity, linearity, accuracy, precision, range, limit of detection, limit of quantitation (LOQ) and robustness. Relative standard deviation (RSD) for system suitability was found 1.3%. Calibration plot was linear over the range of 0.050–2.000 μg/mL. Limit of detection and limit of quantification were found 0.017 and 0.051 μg/mL, respectively. The intra- and inter-day precision RSD was 2.3% and the obtained recovery at LOQ to 200% was in between 86.7 and 107.4%. Conclusion The low RSD values and high recoveries of the method confirm the suitability of the method.

scholarly journals Rapid detection of dimethyl yellow dye in curry by liquid chromatography-electrospray-tandem mass spectrometry

2010 ◽  
Vol 28 (No. 5) ◽  
pp. 427-432 ◽  
Author(s):  
F. Tateo ◽  
M. Bononi ◽  
F. Gallone
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Mass Spectral ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
High Degree ◽  
Positive Ion

An accurate and rapid method, was devised for the identification and quantitation of dimethyl yellow dye in curry, based on liquid chromatography-tandem mass spectrometry interfaced with electrospray. Mass spectral acquisition was done in positive ion mode applying two fragmentation transitions to provide a high degree of selectivity. The extraction system provided a very high recovery (100.0% to 105.8%) and good results were obtained for the limit of detection (5 μg/kg) and limit of quantitation (16 μg/kg). The applicability of the method to identifing and quantifing the unauthorised dimethyl yellow dye in curry was demonstrated.

scholarly journals Dried Urine Microsampling Coupled to Liquid Chromatography—Tandem Mass Spectrometry (LC–MS/MS) for the Analysis of Unconjugated Anabolic Androgenic Steroids

Molecules ◽  
2020 ◽  
Vol 25 (14) ◽  
pp. 3210 ◽  
Author(s):  
Michele Protti ◽  
Camilla Marasca ◽  
Marco Cirrincione ◽  
Angelo E. Sberna ◽  
Roberto Mandrioli ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Anabolic Androgenic Steroids ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Androgenic Steroids

Testing and monitoring anabolic androgenic steroids in biological fluids is a key activity in anti-doping practices. In this study, a novel approach is proposed, based on dried urine microsampling through two different workflows: dried urine spots (DUS) and volumetric absorptive microsampling (VAMS). Both techniques can overcome some common drawbacks of urine sampling, such as analyte instability and storage and transportation problems. Using an original, validated liquid chromatography–tandem mass spectrometry (LC-MS/MS) method, exogenous and endogenous unconjugated steroids were analysed. Despite the limitations of microsampling volume, good sensitivity was obtained (limit of quantitation ≤1.5 ng/mL for all analytes), with satisfactory precision (relative standard deviation <7.6%) and absolute recovery (>70.3%). Both microsampling platforms provide reliable results, in good agreement with those obtained from urine.

scholarly journals Multi-Class Determination of 64 Illicit Compounds in Dietary Supplements Using Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (19) ◽  
pp. 4399
Author(s):  
Dasom Shin ◽  
Hui-Seung Kang ◽  
Hyungsoo Kim ◽  
Guiim Moon
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Dietary Supplements ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

In this work, liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated for screening and confirmation of 64 illicit compounds in dietary supplements. The target compounds were illegally used pharmaceutical drugs, prohibited compounds, and not authorized ingredients for different therapeutics (sexual enhancement, weight loss, muscular strengthening, and relaxing products). The validation procedure was performed to evaluate selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was >0.98 in the range of 0.5–200 µg L−1. The LOQs were in the range 1–10 µg kg−1 for all target compounds. The accuracy (expressed as recovery) was 78.5–114%. The precision (expressed as the relative standard deviation) was below 9.15%. The developed method was applied for the determination of illicit compounds in dietary supplements collected from websites. As a result, the total detection rate was 13.5% (27 samples detected in 200 samples). The concentrations of detected samples ranged from 0.51 to 226 mg g−1. The proposed methodology is suitable for monitoring the adulteration of illicit compounds in dietary supplements.

scholarly journals Determination of Cyclamate in Foods by Ultraperformance Liquid Chromatography/Tandem Mass Spectrometry

2008 ◽  
Vol 91 (5) ◽  
pp. 1095-1102 ◽  
Author(s):  
Robert Sheridan ◽  
Thomas King
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Abstract A highly sensitive and selective method that requires minimal sample preparation was developed for the confirmation and quantitation of cyclamate in a variety of foods by high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Sample preparation consisted of homogenization followed by extraction and dilution of cyclamate with water. HPLC separation was achieved using a bridged ethyl hybrid C18 high-pressure column with a mobile phase consisting of 0.15 acetic acid and methanol. Under electrospray ionization negative conditions, quantitation was achieved by monitoring the fragment m/z 79.7 while also collecting parent ion m/z 177.9. Two food matrixes, diet soda and jelly, were subjected to a validation procedure in order to evaluate the applicability of the method. The cyclamate limit of detection for both matrixes was determined to be 0.050 g/g with a limit of quantitation of 0.150 g/g. The correlation coefficient of the calibration curves was &gt;0.9998 from 0.0005 to 0.100 g/mL. The method has been used for the determination of cyclamate in several foods and the results are presented.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR ANALYSIS OF DEOXYARBUTININ ANHYDROUS EMULSION SYSTEM USING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2019 ◽  
pp. 172-175 ◽  
Author(s):  
MUCHTARIDI MUCHTARIDI ◽  
IDA MUSFIROH ◽  
AHMAD FAUZI
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Emulsion System ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: The aim of this study is to develop a simple, precise and accurate analytical method of deoxyarbutin in anhydrous emulsion system preparation. Methods: The analysis was conducted using high-performance liquid chromatography (HPLC). Chromatographic analysis was carried out using a reversed phase-C18 column. The mobile consists of two phases methanol and water (60: 40 v/v) at a flow rate of 1.0 ml/min. The determinations were performed using UV detector set at 225 nm. All validation procedures were added with hydroquinone as an internal standard. Results: The method showed coefficient correlation is 0.9978, relative standard deviation (RSD) smaller than 2%, Limit of Detection (LOD) and Limit of Quantitation (LOQ) are 0.599 µg/ml and 1.817 µg/ml respectively. The total amount deoxyarbutin in anhydrous emulsion preparation is 1.964+0.02 % with 98% recovery percentage. Conclusion: The developed HPLC analytical method meets the validation criteria made by International Conference on Harmonisation (ICH).

scholarly journals Determination of Diazepam in Cream Biscuits by Liquid Chromatography

2004 ◽  
Vol 87 (3) ◽  
pp. 569-572 ◽  
Author(s):  
Priyankar Ghosh ◽  
Mudiam Mohanakrishna Reddy ◽  
Beedu Sashidhar Rao ◽  
Rajendra Kumar Sarin
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Internal Standard ◽  
Reversed Phase ◽  
Calibration Plot ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract An analytical procedure was developed for the detection and quantitation of diazepam in cream biscuits, which were used to commit crime. The method involves the extraction of diazepam with ethanol at room temperature, and the extract is filtered, evaporated to dryness, and redissolved in the mobile phase, methanol–acetonitrile–tetrahydrofuran–water (15 + 55 + 4 + 26, v/v). The separation is achieved on a C18 reversed-phase column with the mobile phase and diode array detection (λmax) at 230 nm. Medazepam is used as the internal standard is for quantification. The calibration plot for the determination of diazepam is based on linear regression analysis (y = 0.6687x + 0.0372; r2 = 0.995). The limit of detection for diazepam in the biscuit samples was estimated as 600 ng/mL. The limit of quantitation for diazepam was estimated as 1.75 μg/mL. The diazepam detected per piece of biscuit was found to be in the range of 0.27–0.45 mg. Pure diazepam was added to biscuit samples at 3 levels (100 and 500 μg/g, and 1 mg/g), and the recoveries were found to be 95%. The mean retention time of diazepam was 2.7 min and that of medazepam (IS) was 4 min. The relative standard deviations of the diazepam level in the biscuit samples were estimated to be 0.4% for retention time and 1.02% for peak area in intraday analysis, whereas the corresponding values were and 0.61 and 2.34% in interday analysis. The method is rapid and reliable for qualitative and quantitative analysis of cream biscuits laced with diazepam, and it can be used by law enforcement laboratories for routine analysis.

Determination of Okadaic Acid and Dinophysistoxins-1 in Mussel by Liquid Chromatography-Tandem Mass Spectrometry

2014 ◽  
Vol 1033-1034 ◽  
pp. 648-651
Author(s):  
Dong Mei Huang ◽  
Yong Fu Shi ◽  
Cong Kong ◽  
Liang Liang Tian ◽  
Xuan Zhang
Keyword(s):  
Liquid Chromatography ◽  
Okadaic Acid ◽  
Tandem Mass ◽  
Mass Spectrometric Method ◽  
Shellfish Poisoning ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Tandem Mass Spectrometric

A liquid chromatography-tandem mass Spectrometric method for the determination of diarrhetic shellfish poisoning including okadaic acid(OA) and dinophysistoxins-1(DTX-1) in mussel. After being extracted using methanol and water(80:20,V/V),The solution was defatted with n-hexane and extracted in chloroform. After being concentrated ,the residue was dissolved with n-hexane and acetone(20:80,V/V).Then the solution was cleaned-up by solid phase extraction(SPE) on an Si cartridge.The analytes were eluted with methanol - acetone(40:60,V/V). The quantitative and confirmatory determination of OA and DTX-1 were performed by MRM mode. OA and DTX-1 were determined in the negative ion mode. The calibration curves were linear. The method was accurate and reproducible, being successfully applied to the monitoring of OA and DTX-1.The recoveries of standard addition levels were 92.5%-96.7%. The relative standard deviations were all below 6.67%. The limit of quantitation (LOQ) for this method as defined by ten times signal to noise was 20μg/kg.

scholarly journals Determination of ligustrazine in rat serum by polymer monolithic micro-extraction combined with ultra high performance liquid chromatography-tandem mass spectrometry

2020 ◽  
Author(s):  
Danling Sun ◽  
Xitian Peng ◽  
Maomin Peng ◽  
Xian Zhang ◽  
Hong Xia ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Performance ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Rat Serum ◽  
Relative Standard ◽  
Polymer Monolith ◽  
Liquid Chromatography Tandem Mass

AbstractThis study focused on developing an effective and environmentally friendly method to measure ligustrazine in rat serum by using polymer monolith micro-extraction (PMME) technique. A poly (methacrylic acid-ethylene glycol dimethacrylate) material was used to extract ligustrazine through hydrophobic and ion-exchange interaction. Qualitative and quantitative analysis was performed by a liquid chromatography and tandem mass spectrometry. After optimization of several PMME conditions, the developed method exhibited excellent extraction performance to the ligustrazine. Good linearity was acquired ranging from 10 to 2,000 ng mL−1, and the limit of detection of the proposed method was 0.14 ng mL−1. The recoveries measured by spiking three different concentrations in rat serum ranged from 82.6 to 95.3%, and excellent precision was found with relative standard deviations (RSDs) less than 8.3% for intra-day and 9.7% for inter-day, respectively. At last, the applicability of the method was further confirmed through continuous monitoring of ligustrazine in rat serum after dosing of ligustrazine tablets to rats.

scholarly journals EVALUATION OF A NOVEL LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY BASED METHOD FOR VITAMIN D ANALYSIS IN BLOOD

2021 ◽  
Vol 71 (4) ◽  
pp. 1355-59
Author(s):  
Sehrish Naz ◽  
Muhammad Aamir ◽  
Zujaja Hina Haroon ◽  
Sobia Irum Kirmani ◽  
Nisar Ahmed ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Vitamin D ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Mass Spectrometer ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Objective: To evaluate a novel liquid chromatography tandem mass spectrometry based method for serum 25 hydroxy vitamin D (D2 and D3 metabolites) analysis. Study Design: Cross sectional validation study. Place and Duration of Study: Department of Chemical Pathology and Endocrinology, Armed Forces Institute of Pathology, Pakistan, from Mar 2019 to Mar 2020. Methodology: Samples were extracted and 25 OH vitamin-D was separated by means of chromatography and finally quantified via mass spectrometer. A quadrupole- tandem mass spectrometer with Electron spray Ionization coupled to high performance liquid chromatography was adopted for detection and quantitation of 25-hydroxyvitamin D2 and D3 in serum. Results: Limit of detection (LOD) was at the level of 2.49 ng/ml and limit of quantitation (LOQ) was estimated to be 3.9 ng/ml for both the metabolites. The correlation coefficient was 0.99. For D3 observed recovery was 98% and 97.5% respectively while for D2 the recovery was calculated to be 97% and 98%. Percentage relative standard deviation (RSD) was 0.8% and 1.3% respectively. This method has an advantage of less matrix effects, minimal cross-reactivity with 24, 25 hydroxy vit D and 25, 26 di-hydroxy vitamin D metabolite than the routinely used antibody-based assays. Conclusion: This LC-MS/MS methodology is sensitive, specific and can quantitate Vitamin D2 and D3 quite efficiently. This method may be employed for vitamin D analysis in clinical laboratories.

scholarly journals Determination of Deltamethrin Residues in Plant Materials by Liquid Chromatography/Tandem Mass Spectrometry with Electrospray Ionization

2006 ◽  
Vol 89 (3) ◽  
pp. 786-796 ◽  
Author(s):  
Dieter Zimmer ◽  
Christiane Philipowski ◽  
Birgit Posner ◽  
Agnes Gnielka ◽  
Edgar Dirr ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Electrospray Ionization ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Abstract This paper describes a selective and sensitive method that uses liquid chromatography/tandem mass spectrometry with positive electrospray ionization (ESI+) for the determination of deltamethrin in a variety of crops. Samples were extracted by conventional high-speed blending. Some samples required no further cleanup; others were cleaned up by gel permeation chromatography, strong cation-exchange cartridges, or partitioning with n-hexane. In the determinative step, the buffered neutral mobile phase, consisting of 10 mM ammonium acetate (pH 6.8) and methanol, and ESI+ provided strong ammonium adduct formation to [M+NH4]+ at m/z 523, and the multiple-reaction monitoring (MRM) transition at m/z 523/281 was used for the quantitation of deltamethrin. A second MRM transition at m/z 525/283 was used for confirmation. The limit of quantitation (LOQ) values were 0.01 mg/kg for edible materials and 0.05 mg/kg for nonedible materials. Mean overall recoveries at the LOQ and the 10-fold LOQ ranged from 73 to 96%, and the relative standard deviations were &lt;10% for all samples materials analyzed.

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