scholarly journals Microwave-Assisted Extraction Coupled with Mass Spectrometry for Determining Five Volatile Compounds from Soy Sauces

2021 ◽  
Vol 2021 ◽  
pp. 1-8
Author(s):  
Kai Xu ◽  
Xun Gao ◽  
Miaomiao Chi ◽  
Kexin Chen ◽  
Yue Zhang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Limit Of Detection ◽  
Soy Sauce ◽  
Food Culture ◽  
Key Factors ◽  
Assisted Extraction ◽  
Relative Standard ◽  
Benzene Toluene ◽  
Extracting Solvent ◽  
Interday Precision

As a popular fermented condiment in oriental countries, soy sauce plays a more and more important role in modern food culture due to its unique smell and delicious taste. With the help of microwave extraction and gas chromatography-tandem mass spectrometry, the sample preparation method is aimed to determine the content of cyclohexane, benzene, toluene, chlorobenzene, and styrene in soy sauce. The method was validated by examining the linearity, accuracy, specificity, precision, the limit of detection, and quantitation. Meanwhile, three key factors have an impact on the efficiency and accuracy of the method including extracting solvent, temperature, and time which were optimized. The result shows that the recoveries of spiked analytes ranged from 80.86% to 105.71%, the relative standard deviation of intraday and interday precision was no more than 12.1% and 12.5%, and the limit of detection and quantitation were 0.25–1.00 ng/mL and 0.50–2.00 ng/mL, respectively. The results also indicated that the proposed method was a simple, reliable, and sensitive approach for the determination trace amount of five harmful volatile organic compounds from soy sauce.

scholarly journals Determination of 7B3 Residues in Cotton Plants by Liquid Chromatography/Mass Spectrometry

2009 ◽  
Vol 92 (1) ◽  
pp. 302-306 ◽  
Author(s):  
Xiao-Jing Yan ◽  
Xiao-Mei Liang ◽  
Yan-Jun Xu ◽  
Shu-Hui Jin ◽  
Dao-Quan Wang
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Cotton Plants

Abstract A method was developed for the determination of 7B3 (12-propyloxyimino-1,15-pentadecanlactam), a novel macrolactam fungicide, by liquid chromatography/mass spectrometry (LC/MS) with positive electrospray ionization (ESI+). The method used a reversed-phase C18 column and acetonitrilewater (60 + 40, v/v) mobile phase. The quick, easy, cheap, effective, rugged, and safe method was used for extraction of 7B3 from cotton plants, which involved the extraction of 10 g homogenized sample with 10 mL acetonitrile, followed by the addition of 4 g anhydrous MgSO4 and 1.0 g NaCl. After centrifugation, 1 mL of the buffered acetonitrile extract was transferred into a tube containing 50 mg primary secondary amine sorbent and 100 mg anhydrous MgSO4. After shaking and centrifugation, the final extract was transferred to an autosampler vial for concurrent analysis by LC/MS. The results of 7B3 determined by LC/MS in the selective ion monitoring mode were linear, and the matrix effect of the method was evaluated. The average recoveries of 7B3 fortified at different levels were within 84.1100.2, and the relative standard deviations were <7.5 for all samples analyzed. The method limit of detection and the limit of quantitation values were 0.03 and 0.1 mg/kg, respectively. The proposed method was successfully applied to determine 7B3 residues in practical samples. This method is sensitive, accurate, reliable, simple, and safe.

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 Simultaneous Determination of 17 Sulfonamides and the Potentiators Ormetoprim and Trimethoprim in Salmon Muscle by Liquid Chromatography with Tandem Mass Spectrometry Detection

2007 ◽  
Vol 90 (1) ◽  
pp. 343-348 ◽  
Author(s):  
Ross A Potter ◽  
B Garth Burns ◽  
Jeffrey M van de Riet ◽  
David H North ◽  
Rozina Darvesh
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Limit Of Detection ◽  
Fish Tissue ◽  
Reversed Phase ◽  
Tandem Mass ◽  
Relative Standard

Abstract A simple, robust method using liquid chromatography/tandem mass spectrometry (LC/MS/MS) for the simultaneous determination of 17 sulfonamides sulfanilamide (SNL), sulfacetamide (SAA), sulfaguanidine (SGD), sulfapyridine (SPY), sulfadiazine (SDZ), sulfathiazole (STZ), sulfamerazine (SMR), sulfamethoxazole (SOZ), sulfamoxole (SXL), sulfisoxazole (SXZ), sulfamethizole (SML), sulfamethazine (SMZ), sulfamethoxypyridazine (SMP), sulfamonomethoxine (SMM), sulfachloropyridazine (SCP), sulfaquinoxaline (SQX), and sulfadimethoxine (SDM) and 2 potentiators ormetoprim (OMP) and trimethoprim (TMP) in fish tissue has been developed. The analytes were extracted from homogenized fish tissue with wateracetonitrile (50 + 50). The extract was clarified by centrifugation and a portion defatted with hexane. The analytes were partitioned into chloroform and evaporated to dryness. The redissolved residue was applied to a C18 reversed-phase column with a wateracetonitrile (0.1% acetic acid) gradient. All of the compounds were completely separated and detected in <10 min at 30°C using LC/MS/MS. Standard curves were linear over the range of 0.02 to 5 ng injected. The limit of detection varied from 0.1 ng/g for SMZ and OMP to 0.9 ng/g for SXL and SOZ. Recoveries varied from 100% for SDM, SOZ, and SQX and 85% for SMR, OMP, and TMP to approximately 30% for SAA. Relative standard deviations for repeat analysis varied from 4% for SMZ and SCP to 23% for SAA.

scholarly journals Gas Chromatography-Tandem Mass Spectrometry Method for Selective Detection of 2-Nitropropane in Mainstream Cigarette Smoke

2019 ◽  
Vol 28 (7) ◽  
pp. 300-309
Author(s):  
Gala M. Chapman ◽  
Juliana Giraldo Junco ◽  
Roberto Bravo Cardenas ◽  
Clifford H. Watson ◽  
Liza Valentín-Blasini
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Tandem Mass Spectrometry ◽  
Cigarette Smoke ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Standard Deviations ◽  
Mainstream Cigarette Smoke

SummaryAlthough 2-nitropropane is a potentially harmful compound present in cigarette smoke, there are few fully-validated, modern methods to quantitate it in mainstream cigarette smoke. We developed an isotope dilution gas chromatography-tandem mass spectrometry (ID-GC-MS/MS) method for the detection of 2-nitropropane in mainstream cigarette smoke. The vapor fraction of mainstream cigarette smoke was collected in inert polyvinyl fluoride gas sampling bags and extracted with hexanes containing isotopically labeled internal standard, then purified and concentrated via solid-phase extraction using a normal phase silica adsorbent and a 100% dichloromethane eluant. This method is sensitive enough to measure vapor phase 2-nitro-propane concentrations in the nanogram range, with a 19 ng per cigarette method limit of detection. Product variability estimated from the analysis of 15 cigarette products yielded relative standard deviations ranging from 5.4% to 15.7%, and estimates of precision from two quality control products yielded relative standard deviations of 9.49% and 14.9%. Under the Health Canada Intense smoking regimen, 2-nitropropane in machine-generated mainstream smoke from 15 cigarette products ranged from 98.3 to 363 ng per cigarette.

scholarly journals Glycoalkaloid Concentration in Alberta Potatoes Determined by Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry

1999 ◽  
Vol 82 (4) ◽  
pp. 908-914 ◽  
Author(s):  
Darcy R Driedger ◽  
Peter Sporns
Keyword(s):  
Mass Spectrometry ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Laser Desorption ◽  
Maldi Mass Spectrometry ◽  
Ionization Mass ◽  
Relative Standard ◽  
Potato Glycoalkaloids ◽  
Matrix Assisted Laser ◽  
Matrix Assisted Laser Desorption

Abstract Matrix-assisted laser desorption and ionization (MALDI) mass spectrometry was used to determine concentrations of individual potato glycoalkaloids in tubers. Samples were extracted with methanol–water and deposited on 2,4,6-trihydroxyacetophenone crystals. Positive ions were analyzed with a MALDI time-of-flight mass spectrometer equipped with a 337 nm laser. Analyte ion intensities relative to an internal standard were used to determine chaconine and solanine concentrations. Calibration curves were prepared by standard additions to potato tuber material. The relative standard deviations (RSDs) of triplicate measurements ranged from 1 to 16%, with an average of 9%. The day-to-day RSD for replicate determinations was 11 %. Recoveries of analyst-prepared spikes (50 μg/g) averaged 104% for chaconine (RSD, 8%) and 98% for solanine (RSD, 4%). The method limit of detection was estimated to be 2 μg/g.

scholarly journals Validated UV-Vis Spectrophotometric Determination of Andrographolide in Herbal Nano-Preparation

2019 ◽  
Vol 31 (9) ◽  
pp. 1985-1988
Author(s):  
Indah Hairunisa ◽  
Muhammad Da'i ◽  
Erindyah Retno Wikantyasning ◽  
Andhika Rizky Gilang Mahaputra ◽  
Normaidah Normaidah ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Picric Acid ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Herbal Products ◽  
Relative Standard ◽  
Acid Reagent ◽  
Interday Precision ◽  
Detection And Quantification

Determination of major bioactive compounds in polyphyto-formulation is important for production of standardized herbal products. A fast, simple and inexpensive method for detection and quantification of andrographolide concentration in nanoemulsion preparations containing a combination of Andrographis paniculata (Burm f.) Ness. and Phyllanthus niruri L. has been developed. Detection and quantification were carried out using UV-vis spectrophotometry analysis with picric acid reagent and NaOH (8:2) in methanol solvents, read at maximum wavelength 479 nm with 22 min of incubation time. Validation was done by determine the parameters such as linearity, intra and interday precision, accuracy, limit of detection (LOD) and limit of quantification (LOQ). The results obtained showed linearity with r = 0.9945 (y = 0.0109x − 0.2066) in the range of 30-80 μg/mL. The accuracy (recovery) varied in the range of 97.15 to 104.42 %. Percentage of relative standard deviation (% RSD) for precision and intermediate precision value were 3.23 and 3.02 % with LOD value 211 μg/mL and the LOQ 705 μg/mL. As a conclusion, this method is suitable to detect andrographolide content in herbal nano-preparation.

scholarly journals Multi-Steps Fragmentation-Ion Trap Mass Spectrometry Coupled to Liquid Chromatography Diode Array System for Investigation of Olaparib Related Substances

Molecules ◽  
2019 ◽  
Vol 24 (5) ◽  
pp. 843 ◽  
Author(s):  
Alaa Khedr ◽  
Soad El-Hay ◽  
Ahmed Kammoun
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Ion Trap ◽  
Limit Of Detection ◽  
Uv Light ◽  
Degradation Products ◽  
Base Hydrolysis ◽  
Diode Array ◽  
Related Substances ◽  
Relative Standard

A high-performance liquid chromatography-diode array-mass spectrometric (LC-DAD-MS) method was developed and validated to investigate the related substances of olaparib (OLA) in bulk form. OLA was exposed to acid–base hydrolysis, boiling, oxidation with hydrogen peroxide, and UV light followed by LC-DAD-MS analysis. OLA and OLA-related substances were simultaneously and quantitatively monitored by DAD at 278 nm and triple quadrupole mass spectrometry (QQQ-MS). The investigated compounds were auto-scanned by an ion trap MS which applied positive and negative modes separately. The fragmentation pathway was confirmed by applying multi-steps fragmentation to identify the resulted cleaved ions and their parent ion. OLA was found to be sensitive to the alkaline hydrolysis and less sensitive to UV light. Two major hydrolytic degradation products, including the protonated molar ions m/z 299 and m/z 367, were identified. Three potential impurities were also characterized. The LC-MS limit of detection (LOD) and limit of quantification (LOQ) were 0.01 and 0.05 ng/µL, respectively. The quantitative results obtained by LC-DAD was comparable with that of LC-QQQ-MS. The proposed method shows good intra-day and inter-day precision with relative standard deviation (RSD) <2%.

scholarly journals Capillary Electrophoresis–Mass Spectrometry with Multisegment Injection and In-Capillary Preconcentration for High-Throughput and Sensitive Determination of Therapeutic Decapeptide Triptorelin in Pharmaceutical and Biological Matrices

Biomedicines ◽  
2021 ◽  
Vol 9 (10) ◽  
pp. 1488
Author(s):  
Juraj Piešťanský ◽  
Ivana Čižmárová ◽  
Ondrej Štefánik ◽  
Michaela Matušková ◽  
Andrea Horniaková ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Capillary Electrophoresis ◽  
Separation Efficiency ◽  
Limit Of Detection ◽  
Analytical Signal ◽  
Clinical Analysis ◽  
Performance Parameters ◽  
Biological Matrices ◽  
Relative Standard

A capillary electrophoresis–tandem mass spectrometry method with a multisegment injection and an in-capillary field-enhanced sample stacking for determination of therapeutic peptide triptorelin in pharmaceutical and biological matrices was developed. The CE separation conditions were optimized in order to obtain maximal separation efficiency, analytical signal intensity and stability, and minimal adsorption of the analyzed peptide onto the capillary wall (1 M formic acid – HFo, pH 1.88). The implementation of the field-enhanced sample injection into CE improved the value of limit of detection 50 times while the multisegment injection increased the sample throughput three times in comparison to a conventional CE approach. The proposed method was characterized by favorable performance parameters, such as linearity (r2 ≥ 0.99), limit of detection (5 ng mL−1 in water matrix, 25 ng mL−1 in plasma matrix), precision (relative standard deviation, 1.5–9.4% for intraday and 2.3–11.9% for interday reproducibility), or accuracy (relative errors in the range of 80–109%). The FDA-validated method was successfully applied to the analysis of triptorelin in the commercial drug Diphereline® 0.1 mg (powder for injection) and in spiked human plasma samples. Favorable performance parameters along with proven application potentialities indicate the usefulness of the proposed method for its routine use in drug quality control laboratories and for clinical analysis, such as determination of triptorelin levels in plasma (for pharmacokinetic study).

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 Determination of Ethyl Carbamate in Commercial Sweetened Sugar Cane Spirit by ESI-MS/MS Using Modified QuEChERS and 18-Crown-6/Trifluoroacetic Acid Spiking Additives

2022 ◽  
Author(s):  
Angélica Tonin ◽  
Camila Poliseli ◽  
Nayane Sinosaki ◽  
Fernanda Martinez ◽  
Oscar Santos ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Aqueous Phase ◽  
Sugar Cane ◽  
Trifluoroacetic Acid ◽  
Limit Of Detection ◽  
Ethyl Carbamate ◽  
Gas Chromatography Mass Spectrometry ◽  
Esi Ms ◽  
Modified Quechers ◽  
Relative Standard

A fast, sensitive, and selective direct injection electrospray tandem mass spectrometry (DI‑ESI‑MS/MS) method that is able to quantify ethyl carbamate in commercial sweetened sugar cane spirit is described. The preparation method uses a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) with potassium carbonate added to sweetened sugar cane spirit to separate the aqueous phase from the ethanol phase. The aqueous phase contains sucrose that suppresses electrospray ionization. Ethyl carbamate supernatant from the ethanol phase is transferred and enriched with 18-crown-6/trifluoroacetic acid additives. The additives sequester metal cations reducing the ionization of sodium and potassium, favoring the detection of ethyl carbamate as sole protonated cations. The method was successfully applied for the quantification of eleven real samples and certified sugar cane spirit demonstrating its applicability for quality control and regulatory analysis. The method showed reliable analytical parameters compared to conventional gas chromatography mass spectrometry (GC-MS) method commonly used for ethyl carbamate analysis. DI-ESI-MS/MS method requires just a fast step sample clean up and presents consistent values for the limit of detection (LOD 48.0 μg L−1) and limit of quantification (LOQ 160.0 μg L−1). Furthermore, the recoveries obtained were close to 100%, with relative standard deviations below 10% of sample certificates.

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