scholarly journals Development of a Method for Rapid Determination of Morpholine in Juices and Drugs by Gas Chromatography-Mass Spectrometry

2018 ◽  
Vol 2018 ◽  
pp. 1-8 ◽  
Author(s):  
Mengsi Cao ◽  
Pingping Zhang ◽  
Yanru Feng ◽  
Huayin Zhang ◽  
Huaijiao Zhu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Sodium Nitrite ◽  
Recovery Rate ◽  
Rapid Determination ◽  
Low Cost ◽  
Extraction Process ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard

A reliable derivatization method has been developed to detect and quantify morpholine in apple juices and ibuprofen with gas chromatography-mass spectrometry. Morpholine can react with sodium nitrite under acidic condition to produce stable and volatile N-nitrosomorpholine derivative. In this experiment, various factors affecting the derivatization and extraction process were optimized, including volume and concentration of hydrochloric acid, quantity of sodium nitrite, derivatization temperature, derivatization time, extraction reagents, and extraction time. The derivative was extracted with dichloromethane and determined by gas chromatography-mass spectrometry. The linearity range of morpholine was 10–500 μg·L−1 with good correlation, and limits of detection (LOD) and limits of quantification (LOQ) were 7.3 μg·L−1 and 24.4 μg·L−1, respectively. Low, medium, and high concentrations of morpholine were added in apple juices and ibuprofen samples to evaluate standard recovery rate and relative standard deviation. The spiked recovery rate ranged from 94.3% to 109.0%, and the intraday repeatability and interday reproducibility were 2.0%–4.4% and 3.3%–7.0%, respectively. The developed method has good accuracy and precision. This quantitative method for morpholine is simple, sensitive, rapid, and low cost and can successfully be applied to analyze the residual morpholine in apple juices and drug samples.

The Determination of Eight Pesticides in Panax notoginseng of Chinese Traditional Medicine Using Solid-Phase Extraction and Gas Chromatography-Mass Spectrometry

2012 ◽  
Vol 485 ◽  
pp. 68-71
Author(s):  
Na Wu ◽  
Yu Da Zhang ◽  
Wei Liu ◽  
Ping Yi ◽  
Ze Feng Wang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Panax Notoginseng ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard

A simple and effective extraction method based on solid-phase extraction (SPE) was developed to determine chlorothalonil, metalaxyl, triadimefon, dimetachlone, procymidone, flumetralin, oxadixyl and iprodione in Panax Notoginseng using gas chromatography-mass spectrometry with selected ion monitoring (GC/MS, SIM). The prepared samples were analysed with GC-MS in the selected ion monitoring mode (SIM) using one target and two or three qualitative ions for each analyte. In the method, hexane - dichloromethane（6:4，v/v）was selected to effectively extract the pesticides from the Panax Notoginseng samples. Solid-phase extraction was carried out using Supelclean ENVI-Carb/NH2 SPE Column with acetonitrile-toluene (3:1, v/v) as the eluted solvent. In the linear range of each pesticide, the correlation coefficient was R2≥0.99. The limit of detection ranged from 0.001 to 0.05 µg.mL-1, average recoveries ranged from 79.80% to 95.00%, with relative standard deviations between 1.96% and 4.32% for all 8 pesticides.They were readily achieved with this method for all tested pesticides.

scholarly journals Determination of Se4+ in Drinkable Water by Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry

2000 ◽  
Vol 83 (5) ◽  
pp. 1082-1086 ◽  
Author(s):  
Maurizio Guidotti
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Tap Water ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Drinkable Water

Abstract A method was developed for the selective determination of Se4+ in drinkable water by solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS). Se4+ was selectively derivatized to ethane, 1,1′-selenobis by reaction with sodium tetraethylborate, extracted by the SPME fiber, and determined by GC/MS. Both headspace (HS)–SPME and direct SPME were studied. The method requires only a few milliliters of sample and 20 min for completion. At 2.0 μg/L concentration, the relative standard deviation was 10.1% for HS–SPME and 9.1% for direct SPME. For HS–SPME, the theoretical detection limit was 81 ng/L and 166 ng/L for direct SPME. The recovery rate was 95%. The method was used to determine Se4+ in 10 tap water samples.

scholarly journals Determination of Hexabromocyclododecane in Expanded Polystyrene and Extruded Polystyrene Foam by Gas Chromatography-Mass Spectrometry

Molecules ◽  
2021 ◽  
Vol 26 (23) ◽  
pp. 7143
Author(s):  
Tianao Mao ◽  
Haoyang Wang ◽  
Zheng Peng ◽  
Taotao Ni ◽  
Tianqi Jia ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase ◽  
Expanded Polystyrene ◽  
Gas Chromatography Mass Spectrometry ◽  
Polystyrene Foam ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Extruded Polystyrene Foam

A gas chromatography-mass spectrometry (GC/MS) method for the determination of hexabromocyclododecane (HBCD) in expanded polystyrene and extruded polystyrene foam (EPS/XPS) was developed. The EPS/XPS samples were ultrasonically extracted with acetone and the extracts were purified by filtration through a microporous membrane (0.22 μm) and solid-phase extraction. The samples were analyzed using a GC/MS using the selected ion monitoring mode. The ions 157, 319 and 401 were selected as the qualitative ions, while ion 239 was chosen as the quantitative ion. An HBCD standard working solution with a concentration range of 1.0–50.0 mg/L showed good linearity. The detection limit of HBCD was 0.5 mg/kg, meeting the LPC limit (<100 or 1000 mg/kg). Six laboratories were selected to verify the accuracy of the method, and 10 samples were tested. The interlaboratory relative standard deviation range was 3.68–9.80%. This method could play an important role in controlling HBCD contamination in EPS/XPS.

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