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Ou H.,China National Tobacco Quality Supervision & Test Center
Se pu = Chinese journal of chromatography / Zhongguo hua xue hui | Year: 2010

N-nitrosonornicotine (NNN), 4-( methylnitrosamino )-1-(3-pyridyl )-1-butanone (NNK), N-nitrosoanatabine (NAT) and N-nitrosoanabasine (NAB) are the most abundant carcinogens identified in tobacco and tobacco smoke. The accurate quantifications of NNN, NNK, NAT and NAB are necessary to evaluate its impact on the public health. A liquid chromatography-electrospray tandem mass spectrometry (LC-ESI MS/MS) method was developed to simultaneously determine NNN, NNK, NAT and NAB in mainstream cigarette smoke. Mainstream smoke was collected in a Cambridge filter pad and then was extracted by 10 mL 100 mmol/L ammonium acetate after 100 microL of mixed deuterated internal standards was added. Then the extract was detected by using positive electrospray ionization on a tandem mass spectrometer in multiple reaction monitoring (MRM) mode. NNN, NNK, NAT and NAB were separated on a Zorbax Eclipse XDB-C18 column with the gradient elution using mobile phase A (0.1% acetic acid in water) and mobile phase B (0.1% acetic acid in methanol). The detection limits for NNN, NNK, NAT and NAB were 0.019, 0.002, 0.008 and 0.007 microg/L, respectively. The recoveries were varied from 84.9% to 104.5% for Chinese Virginia cigarettes and the relative standard deviations (n = 8) ranged from 2.96% to 6.65%. This proposed approach, which provides a higher sensitivity and specificity, is suitable for the determination of NNN, NNK, NAT and NAB in mainstream cigarette smoke.


Li X.,China National Tobacco Quality Supervision & Test Center | Pang Y.,China National Tobacco Quality Supervision & Test Center | Zhu F.,China National Tobacco Quality Supervision & Test Center | Jiang X.,China National Tobacco Quality Supervision & Test Center | And 3 more authors.
Tobacco Science and Technology | Year: 2015

A method for determining six heavy metal elements, Cr, Ni, As, Se, Cd and Pb, in sidestream cigarette smoke (SCS) was developed by inductively coupled plasma mass spectrometry (ICP-MS). The particulate matter in SCS was collected by a "fishtail" chimney connected with a quartz fiber filter pad, and the gas phase in SCS was trapped by three cascade impingers containing nitric acid, then subjected to microwave digestion, and determined by ICP-MS. The results showed that the correlation coefficients of the calibration curves of the six elements were all above 0.999, and the detection limits ranged from 0.3 to 1.8 ng/cig with the recoveries of 94.0%-109.5%. This method is accurate, sensitive and suitable for the rapid determination of the said heavy metal elements in SCS. ©, 2015, Editorial Office of Tobacco Science and Technology. All right reserved.


Liu Y.,China National Tobacco Quality Supervision & Test Center | Hu J.,CAS Zhengzhou Research Institute | Liu F.,CAS Zhengzhou Research Institute | Zhao M.,CAS Zhengzhou Research Institute | And 2 more authors.
Tobacco Science and Technology | Year: 2015

In order to quantitatively characterize the micro-porous structure of different kind tobacco leaves, the specific surface area and porosity of flue-cured, burley and oriental tobacco leaves were measured by N2-adsorption-desorption-method followed the pretreatment of immersing in ethanol. Meantime, the surface morphology of tobacco samples was observed by a scanning electron microscope (SEM). The results showed that: all the samples possessed obvious characters of porous medium, i.e. larger specific surface area and smaller pore volume; the porosity of oriental tobacco sample was 2.60%, that of flue-cured and burley tobacco samples was 4.78% and 10.73%, respectively; with a higher proportion of pore in leaf, burley tobacco leaf was open in structure; while oriental leaf was relatively close, and flue-cured tobacco leaf was in-between. The pore distribution characters and pore volume of samples agreed with the observation by scanning electron microscope. ©, 2015, Editorial Office of Tobacco Science and Technology. All right reserved.


Pang Y.,China National Tobacco Quality Supervision & Test Center | Jiang X.,China National Tobacco Quality Supervision & Test Center | Luo Y.,China National Tobacco Quality Supervision & Test Center | Li X.,China National Tobacco Quality Supervision & Test Center | And 2 more authors.
Tobacco Science and Technology | Year: 2015

In order to investigate the puff-by-puff release characteristics of mainstream cigarette smoke, a photo-ionization-time-of-flight mass spectrometry (PI-TOF/MS) method was developed for on-line analyzing seven organic compounds (acetaldehyde, 1, 3-butadiene, acetone, isoprene, 2-butanone, benzene and toluene) in mainstream cigarette smoke. The constant volume sampling of mainstream cigarette smoke was achieved by a constant flow orifice, the smoke was directly introduced into the ion source of PI-TOF/MS through a sampling tube with a heating unit. The results showed that: 1) The intra-day and inter-day repeatabilities were good with the relative standard deviations (RSDs) less than 15%, exclusive of the first and the last puffs, where the deviations were larger due to cigarette lighting and variable puff volume, respectively. 2) The RSDs between the results of 1R5F and 3R4F reference cigarettes determined by this method and the mean test values of CORESTA collaborative experiments were less than 10%. 3) The deliveries of different compounds in single puff differed obviously, as did the deliveries between different puffs. This method is simple, fast, accurate, and suitable for the on-line puff-by-puff analysis of mainstream cigarette smoke. ©, 2015, Editorial Office of Tobacco Science and Technology. All right reserved.


Bian Z.,China National Tobacco Quality Supervision & Test Center | Liu S.,China National Tobacco Quality Supervision & Test Center | Yang F.,China National Tobacco Quality Supervision & Test Center | Li Z.,China National Tobacco Quality Supervision & Test Center | And 2 more authors.
Tobacco Science and Technology | Year: 2015

In order to determine the acidity of triacetin efficiently, a rapid titration method was developed with electric continuous liquid divider, and the acidity of 10 domestic and imported triacetin samples was determined. The results showed that: 1) The optimized procedure was as follows: triacetin sample was diluted by anhydrous ethanol, phenolphthalein was added as an indicator, then 0.11 mL of 0.02 mol/L NaOH solution was added quickly by an electric continuous liquid divider at the rate of 0.11 mL every dose repeatedly until solution's color turned pink, the total dose number of NaOH solution addition could be directly translated into triacetin acidity by a conversion table. 2) The recoveries of the method ranged from 99.3% to 99.6% with the relative standard deviations (RSDs) less than 7%. 3) Among the 10 tested samples, the acidity of 7 samples was below the restrictive value of 0.010%, and that of 3 samples was above the value, in which the acidity of 2 samples was more than 0.020%. This method is simple, fast, accurate, and suitable for determining the acidity of triacetin for cigarette. ©, 2015, Editorial Office of Tobacco Science and Technology. All right reserved.


Zhu F.,China National Tobacco Quality Supervision & Test Center | Li X.,China National Tobacco Quality Supervision & Test Center | Luo Y.,China National Tobacco Quality Supervision & Test Center | Pang Y.,China National Tobacco Quality Supervision & Test Center | And 3 more authors.
Tobacco Science and Technology | Year: 2015

In order to investigate the effects of cigarette paper properties on the migration ratios of heavy metal elements in mainstream and sidestream cigarette smoke, 13 cigarette samples were prepared according to single factor design, the effects of permeability, grammage and combustion improver content of cigarette paper on the migration ratio of Cr, Ni, As, Se, Cd and Pb were studied. The results showed that: 1) The air permeability of cigarette paper significantly positively correlated to the migration ratio of Cd in sidestream cigarette smoke in the range of 20-80 CU, while significantly negatively correlated to the migration ratios of As, Cd and Pb in mainstream cigarette smoke in the range of 20-50 CU. 2) The grammage of cigarette paper significantly positively correlated to the migration ratio of Cd in sidestream cigarette smoke, and had no obvious correlations with the migration ratios of the other elements. 3) The content of combustion improver in cigarette paper significantly negatively correlated to the migration ratios of Cr and As in mainstream cigarette smoke and that of As in sidestream cigarette smoke. In conclusion, cigarette paper properties have some, but not the same, effects on the migration ratios of Cr, Ni, As, Se, Cd and Pb in mainstream and sidestream cigarette smoke. ©, 2015, Editorial Office of Tobacco Science and Technology. All right reserved.


Chen H.,China National Tobacco Quality Supervision & Test Center | Jiang X.,China National Tobacco Quality Supervision & Test Center | Wang Y.,China National Tobacco Quality Supervision & Test Center | Zhang W.,China National Tobacco Quality Supervision & Test Center | And 3 more authors.
Tobacco Science and Technology | Year: 2015

To find out the relationships between filter ventilation rate and the deliveries of harmful components in mainstream cigarette smoke under different smoking regimes, the correlations between filter ventilation rate and the deliveries of nicotine and 13 harmful components (acetaldehyde, acrolein, benzene, benzo[a]pyrene, 1,3-butadiene, CO, formaldehyde, NNN, NNK, phenol, crotonaldehyde, HCN and NH3) in mainstream cigarette smoke under ISO and Health Canada intensive (HCI) smoking regimes were investigated, and the correlations between filter ventilation rate and the deliveries of harmful components per unit nicotine yield were analyzed as well. The results showed that: 1) Under ISO smoking regime, filter ventilation rate negatively correlated to the deliveries of harmful components (excluding NNN and NNK); filter ventilation rate negatively correlated to the deliveries of formaldehyde and crotonaldehyde per unit nicotine yield, while positively correlated to the deliveries of acetaldehyde, CO, benzo[a]pyrene and NH3 per unit nicotine yield. 2) Under HCI smoking regime, filter ventilation rate negatively correlated to the deliveries of formaldehyde, crotonaldehyde, benzo[a]pyrene, phenol and nicotine, while positively correlated to the delivery of HCN, there was no significant correlation between filter ventilation rate and the deliveries of the other harmful components. The deliveries of acetaldehyde, acrolein, crotonaldehyde, CO, HCN and NH3 per unit nicotine yield also positively correlated to filter ventilation rate. © 2015, Editorial Office of Tobacco Science and Technology. All right reserved.


PubMed | CAS Hefei Institutes of Physical Science and China National Tobacco Quality Supervision & Test Center
Type: | Journal: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences | Year: 2015

1,3-Butadiene (BD) is a ubiquitous environmental pollutant found in tobacco smoke. In vivo, BD is mainly metabolized to form monohydroxybutenylmercapturic acid (MHBMA) and N-acetyl-S-(3, 4-dihydroxybutyl) cysteine (DHBMA). The accurate quantification of MHBMA and DHBMA in urine may provide important insights into the actual internal exposure of the general population to BD. 8-Hydroxy-2-deoxyguanosine (8-OHdG) is the biomarker of oxidative damage. In this study, a column-switching LC-MS/MS method was developed and validated for the simultaneous quantification of MHBMA, DHBMA derived from BD exposure and 8-OHdG in human urine. Urine samples were loaded on a LiChrospher() RP-8 ADS (25m) 254mm RAM column for the extraction and clean-up of analytes. The separation was achieved using a SUPELCO() LC-18-DB column (75mm3.0mm, 3m). The analytes were ionized in negative electrospray ionization mode and analyzed in multiple reaction monitoring mode. Under optimum conditions, recoveries ranged from 78.9% to 101.7%, with relative standard deviations less than 11%. The limits of quantification ranged from 0.15 to 0.27ng/mL, highlighting the high sensitivity of this simple method. The validated method was successfully applied to analysis urine samples from 56 non-smokers and 233 smokers who smoked cigarettes with 3 different tar yields. There was a correlation between urinary MHBMA, DHBMA and 8-OHdG. This method did not require any preparation process and efficiently removed interference from the matrix by using column-switching. The developed method is applicable to epidemiological studies.


PubMed | CAS Hefei Institutes of Physical Science and China National Tobacco Quality Supervision & Test Center
Type: | Journal: Journal of separation science | Year: 2015

A stable isotope dilution liquid chromatography with tandem mass spectrometry method for the analysis of 16 polycyclic aromatic hydrocarbons in cigarette smoke condensate was developed and validated. Compared with previously reported methods, this method has lower limits of detection (0.04-1.35 ng/cig). Additionally, the proposed method saves time, reduces the number of separation steps, and reduces the quantity of solvent needed. The new method was applied to evaluate polycyclic aromatic hydrocarbon content in 213 commercially available cigarettes in China, under the International Standardization Organization smoking regime and the Health Canadian intense smoking regime. The results showed that the total polycyclic aromatic hydrocarbon content was more than two times higher in samples from the Health Canadian intense smoking regime than in samples from the International Standardization Organization smoking regime (1189.23 vs. 2859.50 ng/cig, p<0.05). Meanwhile, the concentration of individual polycyclic aromatic hydrocarbons (and total polycyclic aromatic hydrocarbons) increased with labeled tar content in both of the tested smoking regimes. There was a positive correlation between total polycyclic aromatic hydrocarbons under the International Standardization Organization smoking regime with that under the Health Canadian intense smoking regime. The proposed liquid chromatography with tandem mass spectrometry method is satisfactory for the rapid, sensitive, and accurately quantitative evaluation of polycyclic aromatic hydrocarbon content in cigarette smoke condensate, and it can be applied to assess potential health risks from smoking. This article is protected by copyright. All rights reserved.


PubMed | Sichuan Tobacco Quality Supervision and Testing Station and China National Tobacco Quality Supervision & Test Center
Type: Journal Article | Journal: Journal of chromatographic science | Year: 2014

A method for the determination of three acidic herbicides, dicamba, 2,4-dichlorophenoxyacetic acid (2,4-D) and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T) in tobacco and soil has been developed based on the use of liquid-liquid extraction and dispersive solid-phase extraction (dispersive-SPE) followed by UPLC-MS/MS. Two percentage of (v/v) formic acid in acetonitrile as the extraction helped partitioning of analytes into the acetonitrile phase. The extract was then cleaned up by dispersive-SPE using primary secondary amine as selective sorbents. Quantitative analysis was done in the multiple-reaction monitoring mode using stable isotope-labeled internal standards for each compound. A separate internal standard for each analyte is required to minimize sample matrix effects on each analyte, which can lead to poor analyte recoveries and decreases in method accuracy and precision. The total analysis time was <4 min. The linear range of the method was from 1 to 100 ng mL(-1) with a limit of detection of each herbicide varied from 0.012 to 0.126 ng g(-1). The proposed method is faster, more sensitive and selective than the traditional methods and more accurate and robust than the published LC-MS/MS methods.

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