scholarly journals Analytical Method for Measurement of Tobacco-Specific Nitrosamines in E-Cigarette Liquid and Aerosol

2018 ◽  
Vol 8 (12) ◽  
pp. 2699 ◽  
Author(s):  
Yoon-Seo Lee ◽  
Ki-Hyun Kim ◽  
Sang Lee ◽  
Richard Brown ◽  
Sang-Hee Jo
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Detection Limit ◽  
Ammonium Acetate ◽  
Tandem Mass ◽  
Average Recovery ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Tobacco Specific Nitrosamines ◽  
Sample Dilution

An experimental method was developed and validated for the collection and analysis of tobacco-specific nitrosamines (TSNAs) that are present in electronic cigarette (EC) liquid or are released from aerosol samples using a liquid chromatography-tandem mass spectrometry (LC-MS/MS) system. As part of this study, the relative recovery of four target TSNAs was assessed by spiking standards in a mixture of propylene glycol and vegetable glycerin. Recovery was assessed against two major variables: (1) the chemical media (solution) selected for sample dilution (acetonitrile [ACN] vs. ammonium acetate [AA]) and (2) the type of sampling filter used (Cambridge filter pad [CFP] vs. quartz wool [QW] tube). The average recovery of TSNAs in terms of variable 1 was 134 ± 22.1% for ACN and 92.6 ± 8.27% for AA. The average recovery in terms of variable 2 was 83.4 ± 7.33% for QW and 58.5 ± 12.9% for CFP. Based on these conditions, the detection limits of N′-nitrosonornicotine (NNN), 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK), N′-nitrosoanatabine (NAT), and N′-nitrosoanabasine (NAB) were calculated as 4.40, 4.47, 3.71, and 3.28 ng mL−1, respectively. The concentration of TSNAs in liquid and aerosol samples of six commercial EC solutions was measured as below the detection limit.

scholarly journals Simultaneous Determination of Cortisol and Cortisone from Human Serum by Liquid Chromatography-Tandem Mass Spectrometry

2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
Sanghoo Lee ◽  
Hwan-Sub Lim ◽  
Hye-Jin Shin ◽  
Seol-A Kim ◽  
Jimyeong Park ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Ammonium Acetate ◽  
Cortisol Concentration ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Cortisol Ratio

A fast, sensitive, and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was validated and then the levels of cortisol and cortisone from sera of healthy adults were determined by the LC-MS/MS method. One hundredμL of serum sample was directly extracted by adding 2 mL ethyl acetate, followed by chromatographic separation on a C18 column with a mobile phase consisting of 5 mM ammonium acetate and methanol (25 : 75, v/v). The precision, accuracy, and average recovery of the method were 1.5–5.3%, 95.4–102.5%, and 96.4% for cortisol, and 1.9–6.0%, 89.2–98.8%, and 79.9% for cortisone, respectively. The method was linear from 1.0 to 500.0 ng/mLr2=0.999for cortisol and 2.5 to 100.0 ng/mLr2=0.998for cortisone. The limits of detection (LOD) and quantification (LOQ) were 0.2 and 1.0 ng/mL for cortisol, and 1.0 and 2.5 ng/mL for cortisone, respectively. The average cortisol concentration (133.9±63.7 ng/mL) of samples collected between 9:00 and 11:00 a.m. was higher approximately 4.4 times than that of cortisone (30.5±10.7 ng/mL)P<0.0001. The average cortisone/cortisol ratio was 0.225. Therefore, the LC-MS/MS method may be useful for the diagnosis of some adrenal diseases and the assessment of 11β-hydroxysteroid dehydrogenase (11β-HSD) activity in clinical laboratories.

Measurement of citrate in urine using liquid chromatography tandem mass spectrometry: comparison with an enzymatic method

2005 ◽  
Vol 42 (5) ◽  
pp. 357-363 ◽  
Author(s):  
BG Keevil ◽  
L Owen ◽  
S Thornton ◽  
J Kavanagh
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Formic Acid ◽  
Ammonium Acetate ◽  
Enzymatic Assay ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Urinary Citrate

Background: Measurement of urine citrate is used to assess the risk of further urinary stone formation and to assess the benefit of treatment in affected individuals. We wanted to develop a simple and rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the analysis of urinary citrate and to compare it with our current enzymatic assay. Methods: For the LC-MS/MS assay, samples were prepared in a deep-well block by adding 10 µL of urine and 20 µL of internal standard to 400 µL of water. After mixing, 3 µL of the diluted sample was injected into the LC-MS/MS system. An LC system was used to isocratically elute a C18 column (50 x 2.1 mm) with 0.4 mL/min water containing 2 mmol/L ammonium acetate and 0.1% (v/v) formic acid. A step gradient of 100% methanol containing 2 mmol/L ammonium acetate and 0.1% (v/v) formic acid was used to wash the column. The retention times were 1.4 min for citrate and 1.4 min for d4-citrate. Cycle time was 4.0 min, injection to injection. The analytes were monitored using a tandem mass spectrometer operated in multiple reaction monitoring mode using the following transitions, citrate m/ z 191.0> 111.0 and d4-citrate m/ z 195.0> 113.0. Results: Within and between-batch coefficients of variation were <3% over the range 480-3800 µmol/L. The lower limit of quantification was 24.0 µmol/L. Regression analysis showed LC-MS/MS = 0.8781 (enzymatic assay) + 102.5, r = 0.964, n = 73. Conclusions: We have developed a simple LC-MS/MS method for urinary citrate measurement that shows acceptable performance.

scholarly journals Determination of prohibited ketone flavors in infant’s cosmetics by high performance liquid chromatography-tandem mass spectrometry

2021 ◽  
Vol 937 (2) ◽  
pp. 022023
Author(s):  
Fengyan Qiu ◽  
Fei Han ◽  
Yanping Hong
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Detection Limit ◽  
Tandem Mass Spectrometry ◽  
Recovery Rate ◽  
Rapid Screening ◽  
Tandem Mass ◽  
Good Precision ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Abstract A rapid screening method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) for five banned ketone fragrances in infant cosmetics has been established. The sample was ultrasonically extracted with acetonitrile, concentrated by nitrogen blowing. Methanol and 0.1% formic acid aqueous solution were used as mobile phases, and separated by gradient elution of HP C18 chromatographic column, and qualitative and quantitative by mass spectrometer. The results showed that the 5 banned ketone fragrances presented a good linear relationship within the mass concentration range of 0.5ug/kg∼50.0ug/kg, and the correlation coefficient r2>0.9983; the detection limit was 0.03ug/kg∼6.25ug/kg, and the limit of quantification is 0.1ug/kg∼ 0.5ug/kg; the average recovery rate of standard addition is between 84.3%∼ 100.6%, and the RSD is between 1.3%∼3.8%. This LC-MS/MS method is suitable for the rapid screening of 5 banned ketone fragrances in complex matrix infant cosmetics, and has the advantages of high recovery rate, low detection limit, and good precision. It can be used to further supplement and improve the technical support for hygiene regulations and quality supervision of banned ketones in cosmetics infant’s cosmetics.

Use of a gas-tight syringe sampling method for the determination of tobacco-specific nitrosamines in E-cigarette aerosols by liquid chromatography-tandem mass spectrometry

2015 ◽  
Vol 7 (11) ◽  
pp. 4472-4480 ◽  
Author(s):  
Young-Hwan Cho ◽  
Ho-Sang Shin
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sampling Method ◽  
Electronic Cigarettes ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Tobacco Specific Nitrosamines ◽  
Gas Tight

We report here a sampling method using a gas-tight syringe (GTS) in the determination of tobacco-specific nitrosamines (TSNAs) in aerosols from electronic cigarettes.

scholarly journals Online In-Tube Solid-Phase Microextraction Coupled to Liquid Chromatography–Tandem Mass Spectrometry for the Determination of Tobacco-Specific Nitrosamines in Hair Samples

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 2056
Author(s):  
Atsushi Ishizaki ◽  
Hiroyuki Kataoka
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tobacco Smoke ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Hair Samples ◽  
Liquid Chromatography Tandem Mass ◽  
Tobacco Specific Nitrosamines

Active and passive smoking are serious public health concerns Assessment of tobacco smoke exposure using effective biomarkers is needed. In this study, we developed a simultaneous determination method of five tobacco-specific nitrosamines (TSNAs) in hair by online in-tube solid-phase microextraction (SPME) coupled to liquid chromatography-tandem mass spectrometry (LC–MS/MS). TSNAs were extracted and concentrated on Supel-Q PLOT capillary by in-tube SPME and separated and detected within 5 min by LC–MS/MS using Capcell Pak C18 MGIII column and positive ion mode multiple reaction monitoring systems. These operations were fully automated by an online program. The calibration curves of TSNAs showed good linearity in the range of 0.5–1000 pg mL–1 using their stable isotope-labeled internal standards. Moreover, the limits of detection (S/N = 3) of TSNAs were in the range of 0.02–1.14 pg mL–1, and intra-day and inter-day precisions were below 7.3% and 9.2% (n = 5), respectively. The developed method is highly sensitive and specific and can easily measure TSNA levels using 5 mg hair samples. This method was used to assess long-term exposure levels to tobacco smoke in smokers and non-smokers.

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