Safety and quality standards for electronic cigarettes (e-cigarettes) have been introduced regionally. In 2016, the U.S. Food and Drug Administration (FDA) issued a rule to regulate e-cigarettes, requiring to report harmful and potentially harmful constituents (HPHCs). In the United Kingdom, the British Standards Institution (BSI) specified the metals to be monitored for e-cigarettes. In this study, a method was developed and validated for the simultaneous determination of 13 metals (Be, Al, Cr, Fe, Co, Ni, Cu, As, Se, Ag, Cd, Sn and Pb) in e-cigarette aerosol. Furthermore, matrix effects of major constituents in the aerosol were investigated using glycerol or 1,2-propylene glycol solutions. E-cigarette aerosol was generated by a rotary smoking machine according to CORESTA Recommended Method N° 81 and collected by an electrostatic precipitator coupled to an impinger containing nitric acid. The collected aerosol was dissolved in nitric acid and an aliquot of this solution was analyzed by inductively coupled plasma mass spectrometry (ICP-MS) equipped with a collision/reaction cell.
The linearity of the calibration curve was observed in the range of 0.2 to 100 ng/mL for each analyte; the correlation coefficients were 0.998 or larger, the mean recovery of each standard level ranged from 92.6 to 104.5% and the relative standard deviation amounted to max. 9.5%. Accuracy, repeatability and specificity were validated by spiking three different amounts of analytes into e-cigarette aerosol; the mean recovery of each spiking level ranged from 88.7 to 110.3% with a relative standard deviation amounting to max. 9.2% for all analytes. Background contamination from aerosol generation and collection system existed for some analytes, especially for Al, Fe, Cu and Sn. The potential sources of contamination should be identified and controlled to reduce the impact of contamination on quantification. In addition, the actual values for samples should be reported with method blank statistics. Increase of the concentrations of glycerol and 1,2-propylene glycol in the prepared sample led to the overestimation of As and Se. The amount of polyols in the collected aerosol should be monitored and controlled for the accurate quantification of As and Se.
Nitrogen (N) fertilization of Kentucky dark fire-cured tobacco can be used to increase weight of high quality cured leaves for cigar manufacture. We conducted field experiments at 11 different locations in the province of Benevento (Southern Italy) where the following four N treatments were compared: 1) unfertilized control (N0); 2) a site-specific N rate, calculated by a N fertilization plan (NFP) based on physical and chemical soil characteristics, which ranged between 113 and 145 kg N ha−1; 3) 200 kg N ha−1 (rate commonly used by farmers, N200); 4) 100 kg N ha−1 (half of the rate commonly used by farmers, N100). Yields of the following five commercial quality categories of cured leaves were measured: i) wrappers, ii) heavy filler (Fh), iii) light filler (Fl), iv) heavy shredded (Sh) and v) light shredded (Sl). Fh cured products of B1, B4, B6 and B10 locations were analyzed for: total alkaloids, reducing sugars, chlorides, total N (Kjeldahl), ammonium-N (NH4-N), nitrate-N (NO3-N), and tobacco specific nitrosamines (TSNA). Color parameters: Lightness (L), Chroma (C) and Hue (H) were determined on five cured leaves / plot of both Fh and Fl types at B1, B2, B3, B6, B8 and B10. A blind evaluation of cured leaves collected across locations was conducted by a panel test who considered the main basic characteristics of cured leaves (stalk position, leaf structure, texture, etc.). The total yield of cured products increased with fertilization across locations, up to NFP treatment, without any statistically significant increase at N200 treatment. Fertilization increased yield of wrappers at B1 up to NFP treatment (113.5 kg N ha−1), without any significant increase at N200 treatment. Yield of light filler product was positively influenced by fertilization up to the maximum dose only in 5 out of 11 locations. Total alkaloids significantly increased with increasing fertilization up to 100 kg N ha−1 without any significant changes at higher N rate. Fertilization hardly increased L and C of Fl leaves, which appeared light-brown but brilliant-colored. There was a reduction in the H value of Fh products which indicated a darker tone of those leaves with respect to Fl. Increasing N rate affected production costs more than revenues. According to agronomic results, in most locations the best results in terms of net revenues were obtained by NFP treatment. Considering that N rates above the NFP would disqualify growers from the economic aids provided by EU agrienvironmental measures, by economic point of view the NFP treatment would be recommended over the current grower standard (N200).
The present study describes the analysis of several organic acids in tobacco and smokeless tobacco products using a liquid chromatography (LC) method with mass spectrometric (MS) detection (LC-MS). Prior to the application of the LC-MS method, a qualitative analysis for the identification of the organic acids in tobacco and oral tobacco products was performed. The qualitative method used direct silylation of the plant material followed by GC-MS separation and detection. For the acids’ quantitation, a novel LC-MS method has been developed and validated. The acids of interest for quantitation were the following: acetic, citric, fumaric, glyceric, lactic, maleic, malic, oxalic, pyroglutamic, pyruvic, quinic, and trihydroxybutanoic. The LC separation was performed on a Synergy 4u Hydro-RP column 250 × 4.6 mm, with an aqueous mobile phase containing 5% methanol and 0.15% formic acid. The LCMS method has the advantage versus LC methods with other detection types (refractive index, UV absorption at low UV range, or conductivity) of being capable of positive identification of the analytes based on their specific ions, and of having significantly better sensitivity. Unfortunately, the LC-MS method was not generating good results for oxalic acid and acetic acid also expected to be present in some samples of tobacco or tobacco products. The study describes the advantages and disadvantages of the LC-MS method for the analysis of organic acids in tobacco and smokeless tobacco products.
In order to investigate the main factors behind hot coal fallout during cigarette smoking, an in-use behavior survey among smokers was conducted in three locations (Guiyang, Shijiazhuang and Nanchang) in China. In addition, a measuring device was designed to record whether a flicking or tapping force was exerted to remove ash and to record the force applied as well as their characteristic parameters. We found that there was no significant difference among the behavior characteristic parameters of the users in the three locations. The proportion of consumers who applied flicking was higher than the proportion of consumers tapping. There were some differences in the in-use behavior when smoking King Size and Superslim cigarettes. The work could help to develop a suitable hot coal fallout test method.
Safety and quality standards for electronic cigarettes (e-cigarettes) have been introduced regionally. In 2016, the U.S. Food and Drug Administration (FDA) issued a rule to regulate e-cigarettes, requiring to report harmful and potentially harmful constituents (HPHCs). In the United Kingdom, the British Standards Institution (BSI) specified the metals to be monitored for e-cigarettes. In this study, a method was developed and validated for the simultaneous determination of 13 metals (Be, Al, Cr, Fe, Co, Ni, Cu, As, Se, Ag, Cd, Sn and Pb) in e-cigarette aerosol. Furthermore, matrix effects of major constituents in the aerosol were investigated using glycerol or 1,2-propylene glycol solutions. E-cigarette aerosol was generated by a rotary smoking machine according to CORESTA Recommended Method N° 81 and collected by an electrostatic precipitator coupled to an impinger containing nitric acid. The collected aerosol was dissolved in nitric acid and an aliquot of this solution was analyzed by inductively coupled plasma mass spectrometry (ICP-MS) equipped with a collision/reaction cell.
The linearity of the calibration curve was observed in the range of 0.2 to 100 ng/mL for each analyte; the correlation coefficients were 0.998 or larger, the mean recovery of each standard level ranged from 92.6 to 104.5% and the relative standard deviation amounted to max. 9.5%. Accuracy, repeatability and specificity were validated by spiking three different amounts of analytes into e-cigarette aerosol; the mean recovery of each spiking level ranged from 88.7 to 110.3% with a relative standard deviation amounting to max. 9.2% for all analytes. Background contamination from aerosol generation and collection system existed for some analytes, especially for Al, Fe, Cu and Sn. The potential sources of contamination should be identified and controlled to reduce the impact of contamination on quantification. In addition, the actual values for samples should be reported with method blank statistics. Increase of the concentrations of glycerol and 1,2-propylene glycol in the prepared sample led to the overestimation of As and Se. The amount of polyols in the collected aerosol should be monitored and controlled for the accurate quantification of As and Se.
Nitrogen (N) fertilization of Kentucky dark fire-cured tobacco can be used to increase weight of high quality cured leaves for cigar manufacture. We conducted field experiments at 11 different locations in the province of Benevento (Southern Italy) where the following four N treatments were compared: 1) unfertilized control (N0); 2) a site-specific N rate, calculated by a N fertilization plan (NFP) based on physical and chemical soil characteristics, which ranged between 113 and 145 kg N ha−1; 3) 200 kg N ha−1 (rate commonly used by farmers, N200); 4) 100 kg N ha−1 (half of the rate commonly used by farmers, N100). Yields of the following five commercial quality categories of cured leaves were measured: i) wrappers, ii) heavy filler (Fh), iii) light filler (Fl), iv) heavy shredded (Sh) and v) light shredded (Sl). Fh cured products of B1, B4, B6 and B10 locations were analyzed for: total alkaloids, reducing sugars, chlorides, total N (Kjeldahl), ammonium-N (NH4-N), nitrate-N (NO3-N), and tobacco specific nitrosamines (TSNA). Color parameters: Lightness (L), Chroma (C) and Hue (H) were determined on five cured leaves / plot of both Fh and Fl types at B1, B2, B3, B6, B8 and B10. A blind evaluation of cured leaves collected across locations was conducted by a panel test who considered the main basic characteristics of cured leaves (stalk position, leaf structure, texture, etc.). The total yield of cured products increased with fertilization across locations, up to NFP treatment, without any statistically significant increase at N200 treatment. Fertilization increased yield of wrappers at B1 up to NFP treatment (113.5 kg N ha−1), without any significant increase at N200 treatment. Yield of light filler product was positively influenced by fertilization up to the maximum dose only in 5 out of 11 locations. Total alkaloids significantly increased with increasing fertilization up to 100 kg N ha−1 without any significant changes at higher N rate. Fertilization hardly increased L and C of Fl leaves, which appeared light-brown but brilliant-colored. There was a reduction in the H value of Fh products which indicated a darker tone of those leaves with respect to Fl. Increasing N rate affected production costs more than revenues. According to agronomic results, in most locations the best results in terms of net revenues were obtained by NFP treatment. Considering that N rates above the NFP would disqualify growers from the economic aids provided by EU agrienvironmental measures, by economic point of view the NFP treatment would be recommended over the current grower standard (N200).
The present study describes the analysis of several organic acids in tobacco and smokeless tobacco products using a liquid chromatography (LC) method with mass spectrometric (MS) detection (LC-MS). Prior to the application of the LC-MS method, a qualitative analysis for the identification of the organic acids in tobacco and oral tobacco products was performed. The qualitative method used direct silylation of the plant material followed by GC-MS separation and detection. For the acids’ quantitation, a novel LC-MS method has been developed and validated. The acids of interest for quantitation were the following: acetic, citric, fumaric, glyceric, lactic, maleic, malic, oxalic, pyroglutamic, pyruvic, quinic, and trihydroxybutanoic. The LC separation was performed on a Synergy 4u Hydro-RP column 250 × 4.6 mm, with an aqueous mobile phase containing 5% methanol and 0.15% formic acid. The LCMS method has the advantage versus LC methods with other detection types (refractive index, UV absorption at low UV range, or conductivity) of being capable of positive identification of the analytes based on their specific ions, and of having significantly better sensitivity. Unfortunately, the LC-MS method was not generating good results for oxalic acid and acetic acid also expected to be present in some samples of tobacco or tobacco products. The study describes the advantages and disadvantages of the LC-MS method for the analysis of organic acids in tobacco and smokeless tobacco products.
In order to investigate the main factors behind hot coal fallout during cigarette smoking, an in-use behavior survey among smokers was conducted in three locations (Guiyang, Shijiazhuang and Nanchang) in China. In addition, a measuring device was designed to record whether a flicking or tapping force was exerted to remove ash and to record the force applied as well as their characteristic parameters. We found that there was no significant difference among the behavior characteristic parameters of the users in the three locations. The proportion of consumers who applied flicking was higher than the proportion of consumers tapping. There were some differences in the in-use behavior when smoking King Size and Superslim cigarettes. The work could help to develop a suitable hot coal fallout test method.