Confirmatory Method for N-Nitrosodimethylamine and N-Nitrosopyrrolidine in Food by Multiple Ion Analysis with Gas Chromatography-Low Resolution Mass Spectrometry Before and After Ultraviolet Photolysis

1982 ◽  
Vol 65 (5) ◽  
pp. 1162-1167
Author(s):  
W I Kimoto ◽  
Walter Fiddler
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Uv Light ◽  
Capillary Gc ◽  
Low Resolution ◽  
Total Extract ◽  
Before And After ◽  
Ultraviolet Photolysis ◽  
Peak Areas ◽  
Volatile Nitrosamines

Abstract A confirmatory procedure is described for determining N-nitrosodimethylamine (NDMA) and N-nitrosopyrrolidine (NPYR) in bacon, beer, and malt by gas chromatography-low resolution quadrupole mass spectrometry (GC-MS). The presence of 3 monitored ions, m/z 30, 42, and 74 for NDMA, and m/z 30,42, and 100 for NPYR, before and disappearance after photolysis under UV light at 365 nm without quantitation of peak areas was considered confirmatory evidence for their presence. The extracts, obtained by mineral oil distillation methods' for bacon and malt, and dry column methods for bacon and beer, underwent cleanup procedures before capillary GC-MS analysis. Less than 100 ng nitrosamine in the total extract, or approximately 2 ng NDMA or 3 ng NPYR injected into the GC-MS instrument, can be confirmed by this method. This technique should also be applicable for other volatile nitrosamines.

Screening and quantification of hypnotic sedatives in serum by capillary gas chromatography with a nitrogen-phosphorus detector, and confirmation by capillary gas chromatography-mass spectrometry.

1986 ◽  
Vol 32 (2) ◽  
pp. 325-328 ◽  
Author(s):  
V A Soo ◽  
R J Bergert ◽  
D G Deutsch
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Capillary Gas Chromatography ◽  
Gas Chromatography Mass Spectrometry ◽  
Detector Response ◽  
Capillary Gc ◽  
Chromatography Mass Spectrometry ◽  
Nitrogen Phosphorus Detector ◽  
Sedative Drugs ◽  
Nitrogen Phosphorus

Abstract We describe a quantitative screen for hypnotic-sedative drugs in which we use capillary gas chromatography with a nitrogen-phosphorus detector (GC/NPD) as the primary method and capillary gas chromatography-mass spectrometry (GC-MS) for confirmation. GC retention times of the acid-extracted underivatized drugs were stable (CVs less than 1%), and the detector response varied linearly over a 20-fold concentration range with a mean correlation coefficient for 11 drugs of 0.989. The limits of detection were satisfactory (0.5 mg/L in a 0.5-mL serum sample and 1-microL injection volume), as were precision (average CV 5.2% within day, 6.4% between day). The complementary use of capillary GC-MS not only unambiguously confirms presumptive peaks identified by GC, but also prevents reports of false positives and identifies compounds not included in the quantitative GC screen that may be listed in the GC-MS library.

scholarly journals Quantitative Analysis and Fingerprint Profiles for Quality Control of Fructus Schisandrae by Gas Chromatography: Mass Spectrometry

2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Yong-Gang Xia ◽  
Bing-You Yang ◽  
Jun Liang ◽  
Qi Yang ◽  
Di Wang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Quality Control ◽  
Assessment Method ◽  
Gas Chromatography Mass Spectrometry ◽  
Active Constituents ◽  
Relative Retention ◽  
Quality Assessment Method ◽  
Peak Areas ◽  
Pharmacologically Active

This paper describes a simple, rapid, and effective quality assessment method for Fructus Schisandrae by gas chromatography-mass spectrum (GC-MS). The method was established by using specific lignan fingerprint profiles and quantitation of characteristic compounds in this herbal medicine. The GC-MS fingerprints of 15 batches ofSchisandrasamples from different regions of China showed similar lignan profiles. Five peaks were selected as characteristic peaks, and all of these were identified by using GC-MS techniques. The relative retention times of these characteristic peaks in the GC-MS fingerprint were established as an important parameter for identification ofSchisandrasamples. Meanwhile, relative peak areas may be a feasible approach to discriminate theS. chinensisandS. sphenanthera. Finally, these pharmacologically active constituents in the titled plant, schisandrins A–C and schizandrols A and B, were quantitatively determined using a validated GC-MS method.

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