Lower limit of detection achieved by raw band-target entropy minimization (rBTEM) for trace and coeluted gas chromatography-mass spectrometry components

2019 ◽  
Vol 52 (10) ◽  
pp. 1579-1589 ◽  
Author(s):  
Bo Lu ◽  
Yunbo Lv ◽  
Fang Li Du ◽  
Chun Kiang Chua ◽  
Hua Jun Zhang
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Lower Limit ◽  
Limit Of Detection ◽  
Gas Chromatography Mass Spectrometry ◽  
Entropy Minimization ◽  
Chromatography Mass Spectrometry

Simultaneous Determination of Alachlor, Metolachlor, Atrazine, and Simazine in Water and Soil by Isotope Dilution Gas Chromatography/Mass Spectrometry

1989 ◽  
Vol 72 (2) ◽  
pp. 349-354 ◽  
Author(s):  
Lee Q Huang
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Isotope Dilution ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry

Abstract A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.

scholarly journals Development of Sensitive and Specific Analysis of Vildagliptin in Pharmaceutical Formulation by Gas Chromatography-Mass Spectrometry

2015 ◽  
Vol 2015 ◽  
pp. 1-7
Author(s):  
Ebru Uçaktürk
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Pharmaceutical Formulation ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry ◽  
Validation Parameters ◽  
Diagnostic Ions

A sensitive and selective gas chromatography-mass spectrometry (GC-MS) method was developed and fully validated for the determination of vildagliptin (VIL) in pharmaceutical formulation. Prior to GC-MS analysis, VIL was efficiently derivatized with MSTFA/NH4I/β-mercaptoethanol at 60°C for 30 min. The obtained O-TMS derivative of VIL was detected by selected ion monitoring mode using the diagnostic ionsm/z223 and 252. Nandrolone was chosen as internal standard. The GC-MS method was fully validated by the following validation parameters: limit of detection (LOD) and quantitation (LOQ), linearity, precision, accuracy, specificity, stability, robustness, and ruggedness. LOD and LOQ were found to be 1.5 and 3.5 ng mL−1, respectively. The GC-MS method is linear in the range of 3.5–300 ng mL−1. The intra- and interday precision values were less than ≤3.62%. The intra- and interday accuracy values were found in the range of-0.26–2.06%. Finally, the GC-MS method was successfully applied to determine VIL in pharmaceutical formulation.

scholarly journals METHOD VALIDATION FOR ORGANOCHLORINE INSECTICIDES DETERMINATION IN GINSENG BY USING ISOTOPE-DILUTION GAS CHROMATOGRAPHY-MASS SPECTROMETRY (ID-GC-MS)

2020 ◽  
Vol 17 (34) ◽  
pp. 362-372
Author(s):  
Yosi ARISTIAWAN ◽  
Dillani PUTRI RAMADHANINGTYAS ◽  
Isna KOMALASARI ◽  
Dyah STYARINI ◽  
Nuryatini HAMIM
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Method Validation ◽  
Isotope Dilution ◽  
Limit Of Detection ◽  
Plant Protection ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Organochlorine Insecticides ◽  
Limit Of Quantitation

Organochlorine insecticides are still exploited among the most prominent pesticides for plant protection purposes. Known for having hazardous to humans and persistent in the environment properties, it is necessary to build an accurate method for detecting organochlorine insecticides in food and environmental substances. Isotope-dilution gas chromatography-mass spectrometry (ID-GC-MS) is a versatile coupling measurement system and high order method that combines both selectivity, sensitivity and high accuracy. The present paper aims at showing the methodology of the organochlorine insecticides (alpha-HCH and gamma-HCH) determination in ginseng by using ID-GC-MS. The described method covered sample preparation using an organic solvent (hexane) extraction, followed by florisil cleaning-up. After the reconstitution of the solvent base, the measurement was conducted by using ID-GC-MS in the optimal instrument parameter. Using the determined optimal conditions, the parameters such as sensitivity, linearity, precision, and accuracy were studied for validation of the ID-GC–MS method. The limit of detection and the limit of quantitation of the instrument were 0.5 ng/g and 2.0 ng/g for both analytes. The method showed linearity with the correlation coefficient of 0.999 for both alpha-HCH and gamma-HCH over the concentration range of 1‒300 ng/g. The precision ranged from 3.0 to 3.7% and 2.4 to 3.3% for alpha-HCH and gamma-HCH, respectively. The mean recoveries for alpha-HCH and gamma-HCH were found at 98.0 and 95.6%, respectively. Following method validation, the measurement uncertainty of the alpha-HCH and gamma-HCH determination was evaluated according to EURACHEM GUM guide at a 95 % confidence level (k = 2). The expanded uncertainty in the measurement of alpha-HCH and gamma-HCH was 5.4% and 8.2%, respectively. All these parameters demonstrate the high sensitivity of the offered method and the success of the described method in the determination of alpha-HCH and gamma-HCH in ginseng sample.

scholarly journals Determination of vinyl chloride monomer in food contact materials by solid phase microextraction coupled with gas chromatography/mass spectrometry

2011 ◽  
Vol 21 (No. 1) ◽  
pp. 13-17 ◽  
Author(s):  
I. Jordáková ◽  
J. Dobiáš ◽  
M. Voldich ◽  
J. Poustka
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Vinyl Chloride ◽  
Solid Phase Microextraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Vinyl Chloride Monomer ◽  
Contact Materials ◽  
Chromatography Mass Spectrometry

The present study concerns the optimisation of the headspace solid phase microextraction (HS/SPME) combined with gas chromatography/mass spectrometry (GC/MS) for the vinyl chloride monomer determination. Samples of PVC materials were analysed using the Carboxen/Polydimethylsiloxane (CX/PDMS) 75 µm fibre. For this fibre, the achieved limit of detection was 0.05 µg/kg, and that of quantification 0.17 µg/kg, respectively, with RSD 5%. The levels of VCM found ranged from 0.29 to 0.44 mg/kg, in the case of foil, the VCM content determined was 3.65 mg/kg which means that the maximal limit allowed was exceeded.  

scholarly journals Determination of Phytosterols in vegetable oils by GC-MS method

2020 ◽  
Vol 3 (4) ◽  
pp. 36-42
Author(s):  
Hien Dang Thu ◽  
Ngoc Anh Mai Thi ◽  
Hong Ngoc Nguyen Thi ◽  
◽  
◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Vegetable Oils ◽  
Limit Of Detection ◽  
Alkaline Media ◽  
Gas Chromatography Mass Spectrometry ◽  
Limit Of Quantification ◽  
Chromatography Mass Spectrometry ◽  
Trimethylsilyl Ethers

In this study, a method for determination of six phytosterols by gas chromatography-mass spectrometry with derivatization in vegetable oils was validated. The samples were hydrolyzed in an alkaline media at 70°C for 60 min. Then, the samples were performed liquid-liquid extraction with toluene. The phytosterols are derivatized to trimethylsilyl ethers and then analyzed by gas chromatography-mass spectrometry. The limit of detection and limit of quantification was 5 and 15 mg/kg, respectively. Recoveries of six phytosterols were between 93.5% and 101%.

scholarly journals Quantitative analysis of arbutin and hydroquinone in strawberry tree (Arbutus unedo L., Ericaceae) leaves by gas chromatography-mass spectrometry / Kvantitativna analiza arbutina i hidrokinona u listovima obične planike (Arbutus unedo L., Ericaceae) plinskokromatografskom metodom uz detekciju masenim spektrometrom

2015 ◽  
Vol 66 (3) ◽  
pp. 197-202 ◽  
Author(s):  
Karlo Jurica ◽  
Irena Brčić Karačonji ◽  
Sandra Šegan ◽  
Dušanka Milojković Opsenica ◽  
Dario Kremer
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Limit Of Detection ◽  
Dry Weight ◽  
Gas Chromatography Mass Spectrometry ◽  
Phenolic Glycoside ◽  
Good Precision ◽  
Arbutus Unedo ◽  
Chromatography Mass Spectrometry ◽  
Strawberry Tree

Abstract The phenolic glycoside arbutin and its metabolite with uroantiseptic activity hydroquinone occur naturally in the leaves of various medicinal plants and spices. In this study, an extraction procedure coupled with gas chromatography-mass spectrometry (GC-MS) was developed to determine arbutin and hydroquinone content in strawberry tree (Arbutus unedo L., Ericaceae) leaves. The method showed good linearity (R2>0.9987) in the tested concentration range (0.5-200 μg mL-1), as well as good precision (RSD<5 %), analytical recovery (96.2-98.0 %), and sensitivity (limit of detection=0.009 and 0.004 μg mL-1 for arbutin and hydroquinone, respectively). The results obtained by the validated GC-MS method corresponded well to those obtained by high performance liquid chromatography (HPLC) method. The proposed method was then applied for determining arbutin and hydroquinone content in methanolic leaf extracts. The amount of arbutin in the leaves collected on the island of Koločep (6.82 mg g-1 dry weight) was found to be higher (tpaired=43.57, tc=2.92) in comparison to the amount of arbutin in the leaves collected on the island of Mali Lošinj (2.75 mg g-1 dry weight). Hydroquinone was not detected in any of the samples. The analytical features of the proposed GC-MS method demonstrated that arbutin and hydroquinone could be determined alternatively by gas chromatography. Due to its wide concentration range, the method could also be suitable for arbutin and hydroquinone analysis in leaves of other plant families (Rosaceae, Lamiaceae, etc.).

scholarly journals Extraction-Free, Direct Determination of Caffeine in Microliter Volumes of Beverages by Thermal Desorption-Gas Chromatography Mass Spectrometry

2020 ◽  
Vol 2020 ◽  
pp. 1-7
Author(s):  
Xianglu Peng ◽  
Melanie Brown ◽  
Paul Bowdler ◽  
Kevin C. Honeychurch
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Thermal Desorption ◽  
Limit Of Detection ◽  
Direct Determination ◽  
Energy Drink ◽  
Gas Chromatography Mass Spectrometry ◽  
Pyrolysis Gas ◽  
Chromatography Mass Spectrometry

An extraction-free method requiring microliter (μL) volumes has been developed for the determination of caffeine in beverages. Using a pyrolysis-gas chromatography mass spectrometry system, the conditions required for the direct thermal desorption-gas chromatography mass spectrometry (TD-GC/MS) determination of caffeine were optimised. A 5 μL aliquot was introduced to the thermal desorption unit, dried, and thermally desorbed to the GC/MS. The response was linear over the range 10 to 500 μg/mL (R2 = 0.996). The theoretical limit of detection (3 σ) was 0.456 μg/mL. No interferences were recorded from endogenous beverage components or from commonly occurring drugs, such as nicotine, ibuprofen, and paracetamol. Replicate caffeine determinations on fortified latte style white coffee and Pepsi Max® gave mean recoveries of 93.4% (%CV = 4.1%) and 95.0% (%CV = 0.98%), respectively. Good agreement was also obtained with the stated values of caffeine for an energy drink and for Coca-Cola®. These data suggest that the method holds promise for the determination of caffeine in such samples.

scholarly journals Procedure for Detecting and Confirming Pentobarbital Residues in Dog Food by Gas Chromatography/Mass Spectrometry

1998 ◽  
Vol 81 (2) ◽  
pp. 359-367 ◽  
Author(s):  
Laura A Adam ◽  
Valerie B Reeves
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Organic Layer ◽  
Chromatography Mass Spectrometry ◽  
Solid Phase Extraction Cartridge ◽  
High Concentrations ◽  
Phosphate Buffered Saline

abstract The method described detects and confirms presence of pentobarbital residues in dry, extruded feeds at concentrations of 5-20 ppb. Dried feed is ground to a uniform powder and shaken overnight in methanol. A portion of the methanolic extract is evaporated, and the residue is reconstituted in phosphate-buffered saline. The aqueous extract is cleaned with a solid-phase extraction cartridge designed to extract barbiturate residues from biological matrixes. Dimethyl sulfoxide, tetramethylammonium hydroxide, and iodomethane are added to derivatize pentobarbital. 1,3-Dimethylpentobarbital is then acidified with dilute hydrochloric acid and extracted with isooctane. The organic layer is transferred and evaporated under a stream of nitrogen. The residue is reconstituted in a small volume of ethyl acetate for analysis by gas chromatography/mass spectrometry. The limit of detection is approximately 0.7 ppb. The method was validated with pentobarbital-fortified feed samples containing high concentrations of meat and bone meal.

scholarly journals A simplified approach for determination of urinary ethyl glucuronide by gas chromatography–mass spectrometry

2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Shayani Ghosh ◽  
Raka Jain ◽  
Satpal Singh ◽  
Ravindra Rao ◽  
Ashwani Kumar Mishra ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Human Urine ◽  
Impact Ionization ◽  
Limit Of Detection ◽  
Extraction Procedure ◽  
Ethyl Glucuronide ◽  
Gas Chromatography Mass Spectrometry ◽  
Limit Of Quantification ◽  
Chromatography Mass Spectrometry

AbstractUrinary ethyl glucuronide (EtG), an alcohol biomarker, plays an essential role in monitoring alcohol abstinence and relapse during treatment for alcohol dependence. Detection of this biomarker has become a routine in many clinical and forensic laboratories over the last few years. Most previously published methods commonly use hyphenated chromatographic techniques along with extensive extraction procedure before analysis. This work aimed to develop and validate an electron impact ionization mode gas chromatography–mass spectrometry method to measure ethyl glucuronide levels in human urine. For its determination, urine samples were dried under a gentle stream of nitrogen, derivatized with N,O-bis(trimethylsilyl) trifluoroacetamide, incubated, and injected into the instrument. The analysis was performed using single quadrupole gas chromatography–mass spectrometry (GC-MS) technology and validation was performed according to the guidelines of the German Society of Toxicology and Forensic Chemistry (GTFCh). The linearity of urinary EtG was obtained in the range of 30–5000 ng/ml with a correlation coefficient (r) above 0.999. The extraction recoveries exceeded 80%, and the obtained inter-day and intra-day precisions were below 15%. The achieved limit of detection was 10 ng/ml and limit of quantification achieved was 30 ng/ml. The electron ionization gas chromatography–mass spectrometry technique proves to be a feasible option for determining EtG in human urine when other sophisticated techniques are unapproachable. This method provides a good sensitivity and proves to be cost-effective, robust, and advantageous for both clinical as well as forensic settings.

scholarly journals Single-Laboratory Validation of a Method for the Determination of Furan in Foods by Using Static Headspace Sampling and Gas Chromatography/Mass Spectrometry

2006 ◽  
Vol 89 (5) ◽  
pp. 1417-1424 ◽  
Author(s):  
Patricia J Nyman ◽  
Kim M Morehouse ◽  
Timothy P McNeal ◽  
Gracia A Perfetti ◽  
Gregory W Diachenko
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Apple Juice ◽  
Limit Of Detection ◽  
Peanut Butter ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract A headspace gas chromatography/mass spectrometry method was developed and validated in-house for the determination of furan in foods. The method of standard additions with d4-furan as the internal standard was used to quantitate furan. The limit of detection and limit of quantitation (LOQ) values ranged from 0.2 and 0.6 ng/g, respectively, in apple juice to 0.9 and 2.9 ng/g, respectively, in peanut butter. Recoveries were obtained at 0.5, 1, 2, and 3 times the LOQ. At 1, 2, and 3 times the LOQ, the recoveries ranged from 89.4 to 108%, and the relative standard deviations ranged from 3.3 to 17.3% for all the matrixes. For apple juice, chicken broth, and infant formula, the averaged coefficients of determination from the linear regression analyses were &gt;0.99 with each food fortified at 0.5, 1, 2, and 3 times the LOQ. The coefficients of determination were &gt;0.99 for green beans and 0.96 for peanut butter with the foods fortified at 1, 2, and 3 times the LOQ. Within-laboratory precision was determined by comparing the amounts of furan found in 18 samples by 2 analysts on different days with different instruments. For most of the foods, the difference between the amounts found by each analyst was &lt;18%. The method was used to conduct a survey of &gt;300 foods. The furan levels found ranged from none detected to 174 ng/g.

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