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In this study, we report a portable kit consisting of a portable workstation, gold screen-printed electrode (SPE), 0.45 μm filter membrane, phosphate buffer solution (PBS), and acetic acid (1%) for point-of-use (POU) analysis of nicotine in tobacco. The activated-screen-printed electrode (A-SPE) displayed superior electron transmission efficiency, and the A-SPE without modification was employed for high-performance analysis of nicotine in actual tobacco after simple sample pretreatment. Remarkably, the fabricated nicotine sensor exhibited a broad working range of 10-100 μg g

In this work, the two-step headspace (HS) technique was applied to determine the actual volatile compositions of tea infusions. In order to eliminate the influence of water vapor to the gas chromatography-mass spectrometry (GC-MS) analysis and enable the capability to determine the volatile compounds in water base samples, a programed temperature vaporizer (PTV) was employed for the additional pre-concentration of thee analytes. While using the reported method, the volatile compounds were retained by the absorbent packed in the PTV, while the water vapor was directly removed through the purge valve. Then the retained volatile compounds were splitlessly injected into the GC column, which means that very low detection limits were achieved with the newly developed method. The obtained results demonstrated that the reported protocol possessed excellent repeatability and stability for volatile compound determination, and a total of 94 volatile compounds were identified from 28 teas. Multivariate data analysis was performed to obtain insights into the relationship between volatile compounds composition of the teas and their types. The volatiles composition of tea was shown to be closely related to the processing techniques adopted. Furthermore, the characteristic volatile compounds of each tea type were also illustrated. All of the results demonstrated that the presented method is a reliable approach to analyze and discriminate various beverages.

Facile construction of 1,3-dienes building upon cross-electrophile coupling of two open-chain vinyl halides is disclosed in this work, showing moderate chemoselectivities between the terminal bromoalkenes and internal vinyl bromides. The present method is mild and tolerates a range of functional groups and can be applied to the total synthesis of a tobacco fragrance solanone.

Two-dimensional (2D) transition metal dichalcogenides (TMDs) like molybdenum diselenide (MoSe 2 ) have recently gained considerable interest since their properties are complementary to those of graphene. Unlike gapless graphene, the band structure of MoSe 2 can be changed from the indirect band gap to the direct band gap when MoSe 2 changed from bulk material to monolayer. This transition from multilayer to monolayer requires atomic-layer-precision thining of thick MoSe 2 layers without damaging the remaining layers. Here, we present atomic-layer-precision thinning of MoSe 2 nanaosheets down to monolayer by using SF 6 + N 2 plasmas, which has been demonstrated to be soft, selective and high-throughput. Optical microscopy, atomic force microscopy, Raman and photoluminescence spectra suggest that equal numbers of MoSe 2 layers can be removed uniformly regardless of their initial thickness, without affecting the underlying SiO 2 substrate and the remaining MoSe 2 layers. By adjusting the etching rates we can achieve complete MoSe 2 removal and any disired number of MoSe 2 layers including monolayer. This soft plasma etching method is highly reliable and compatible with the semiconductor manufacturing processes, thereby holding great promise for various 2D materials and TMD-based devices.

Nicotine (Nic) exposed to the environment which comes from tobacco products is the main addictive agent and specific classes of hazardous compound that merit concern. In this study, we have established a fast and reliable method to achieve specific detection of Nic in natural nicotiana tabacum within 30 s through a miniaturized platform based on screen printed gold electrode (SPE). A simple electrochemical pretreatment mean was employed on gold surface that led to the exposure of Au (111) facet and a convenient sample pretreatment method was adopted to realize the extraction of Nic in tobacco. The present electrochemical sensor exhibits an ample range of sensing from 10 μg/g to 200 μg/g, which is able to compliance with tobacco industry testing standards of actual samples. Over 60 sampling points from different origins in China or other countries were performed with direct analysis using this method and satisfactory results have been obtained. The proposed approach was demonstrated to be a very promising platform for significantly improving analytical efficiency in laboratories as well as for monitoring the source reduction control of Nic in the environment.

Solvent microextraction (SME), such as single-drop microextraction (SDME), hollow-fiber liquid-phase microextraction (HF-LPME) and dispersive liquid-liquid microextraction (DLLME), has been explored for its ability to cover a wide range of analytes. Microextraction, combined microextraction with derivatization can greatly improve separation, detectability and compound identification, expand its scope of application, and improve the effect of analysis. In this view, the article not only highlights the development of the microextraction technology such as SDBE, HF-LPME and DLLME, but also improves the key strategies of microextraction coupled to derivatization in analytical chemistry. In order to encourage further development of microextraction-derivatization, its coupling with different analytical techniques such as GC or GC-MS, HPLC, and the other technique has also been discussed.

In this work, for the first time, headspace (HS) single-drop microextraction and simultaneous derivatization followed by GC-MS was developed to determine the aliphatic amines in tobacco samples. In the HS extraction procedure, the mixture of derivatization reagent and organic solvent was employed as the extraction solvent for HS single-drop microextraction and in situ derivatization of aliphatic amine in the samples. Fast extraction and simultaneous derivatization of the analytes were performed in a single step, and the obtained derivatives in the microdrop extraction solvent were analyzed by GC-MS. The optimized experiment conditions were: sample preparation temperature of 80°C and time of 30 min, HS extraction solvent (the mixture of benzyl alcohol and 2,3,4,5,6-pentafluorobenzaldehyde) volume of 2.0 μL, extraction time of 90 s. With the optimal conditions, the method validations were also studied. The method has good linearity (R2 more than 0.99), accepted precision (RSD less than 13%), good recovery (98–104%) and low limit of detection (0.11–0.97 μg/g). Finally, the proposed technique was successfully applied to the analyses of aliphatic amines in tobacco samples of seven different brands. It was further demonstrated that the proposed method offered a simple, low-cost and reliable approach to determine aliphatic amines in tobacco samples.

In this work, the novel technique based on headspace single-drop microextraction with in-syringe derivatization followed by GC-MS was established to determine the volatile organic acids in tobacco. The parameters for headspace single-drop microextraction and in-syringe derivatization were optimized, including extraction time, and volume of derivatization reagent and in-syringe derivatization time. The method validations including linearity, precision, recovery and LOD were also studied. The obtained results illustrated that the optimized technique was easy, highly efficient and sensitive. Finally, the proposed method was successfully applied to the analyses of volatile organic acids in tobacco samples with seven different brands. It was further demonstrated that the present technique developed in this study does offer a simple and fast approach to determine volatile organic acids in tobacco.

Ergosterol is one of the important precursors of tumorigenic polynuclear aromatic hydrocarbons. A large amount of ergosterol is present in mildewy cigarettes, which derives from fungal contaminations. In this paper, a novel approach based on C(18)-functionalized magnetic silica nanoparticles (C(18)-f-MS NPs) coupled with microwave-assisted derivatization and gas chromatography/mass spectrometry (GC/MS) was developed for the rapid enrichment and determination of ergosterol in cigarettes. Due to that, microwave-assisted derivatization requires very short time (several minutes), and the extraction and concentration of ergosterol become the key step in the sample preparation process. In this study, the prepared C(18)-f-MS NPs with its unique properties (high surface area and strong magnetism) provided an efficient way for extraction and concentration of ergosterol in the samples. Additionally, the analyte of ergosterol adsorbed with C(18)-f-MS NPs in cigarettes can be simply and rapidly isolated (only about 2s) through placing a strong magnet on the bottom of container. In this work, different parameters such as added amounts of C(18)-f-MS NPs, extraction temperature, and extraction time were optimized to enhance the extraction efficiency. Method validations (linear range, detection limit, precision, and recovery) were also studied. The results obtained by the optimal conditions showed that the proposed method based on C(18)-f-MS NPs was a simple, high efficient, and had a rapid approach for the enrichment of ergosterol in cigarettes and was successfully applied to the analysis of ergosterol in normal and mildewy cigarettes followed by microwave-assisted derivatization and GC/MS.

Ergosterol is one of the important precursors of tumorigenic polynuclear aromatic hydrocarbons. To the best of our knowledge, a large amount of ergosterol is present in moldy cigarettes, which derives from fungal contaminations. Thus, the development of a simple, fast, and efficient method for the analysis of ergosterol is in great demand. In this paper, GC/MS following microwave-assisted silylation (MAS) was developed for the rapid quantitative analysis of ergosterol in cigarettes for the first time. In our work, total ergosterol in cigarettes after NaOH saponification was extracted with hexane, and then was fast derivatized with bis(trimethylsilyl)trifluoroacetamide (BSTFA) under microwave irradiation. Finally, the ergosterol trimethylsilyl derivative was analyzed by GC/MS. Derivatization conditions including microwave reaction solvent, irradiation time, and power were investigated. Method validations (linear range, LOD, precision, and recovery) were also studied. The results showed that the proposed method provided a fast, simple, and sensitive approach for the determination of ergosterol in cigarettes. Finally it was successfully applied to the analysis of ergosterol in normal and mildewy cigarettes.

A sensitive and reliable high-performance liquid chromatographic method was developed for the determination of vertilmicin in rat plasma. Derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl) followed by C 18 reversed-phase chromatography allowed the fluorimetric detection of vertilmicin. Optimal conditions for the derivatization of vertilmicin are described. The limit of quantification was 0.02 mg/L. The pharmacokinetics of vertilmicin was studied in 24 rats following intramuscular injection (i.m.) of different doses (4, 8, 16, 32 mg/kg of body weight). The pharmacokinetic parameter values were estimated by use of 3P97 program. In this study, we assessed the dose proportionality of vertilmicin after single intramuscular injection doses and obtained new information on the pharmacokinetics of the compound.

Four sampling techniques, solid-phase microextraction (SPME), supercritical fluid extraction (SFE), steam distillation (SD), and solvent extraction (SE), were compared for the analysis of volatile constituents from a traditional Chinese medicine (TCM) of the dried ripe fruit of Fructus Amomi (Sha Ren). A total of 38 compounds were identified by gas chromatography/mass spectrometry. Different SFE and SPME parameters (modifier content, extraction pressure, and temperature for SFE and fibers, extraction temperature, and time for SPME) were studied. The results by SFE and SPME were compared with those obtained by conventional SD and SE methods. The results showed that SFE and SPME are better sample preparation techniques than SD and SE. Due to SFE's requirement for expensive specialized instrumentation, the simplicity, low cost, and speed of SPME make it a more appropriate technique for extraction of volatile constituents in TCMs.

A simple, rapid and sensitive method for determination of rivastigmine in plasma samples was developed using headspace solid-phase microextraction (HS-SPME) and gas chromatography with mass spectrometry (GC–MS). The optimum conditions for the SPME procedure were: headspace extraction on a 65-μm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber; 0.5 ml of plasma modified with 1.0 ml of sodium hydroxide-sodium carbonate solution (0.7 M:0.5 M); extraction temperature of 100 °C, with stirring at 2000 rpm for 30 min. The calibration curve showed linearity in the range from 0.2 to 80 ng/ml with regression coefficient corresponding to 0.9965 and coefficient of the variation of the points of the calibration curve lower than 10%. The quantification limit for rivastigmine in plasma was 0.2 ng/ml. The method was applied to determination of rivastigmine in canine plasma samples from animals after a single oral administration.

In this study, a novel fully automated on-line coupled liquid chromatography-gas chromatography (LC-GC) technique was reported and applied for the determination of organochlorine pesticide residues (OCPs) in tobacco and tobacco products. Using a switching valve to isolate the capillary pre-column and the analytical column during the solvent evaporation period, the LC solvent can be completely removed and prevented from reaching the GC column and the detector. The established method was used to determinate the OCPs in tobacco samples. By using Florisil SPE column and employing GPC technique, polarity impurities and large molecule impurities were removed. A dynamic range 1-100ng/mL was achieved with detection limits from 1.5 to 3.3μg/kg. The method exhibited good repeatability and recoveries. This technology may provide an alternative way for trace analysis of complex samples.

Acetaldehyde is regarded as a toxic mainstream cigarette smoke constituent, and measurement of acetaldehyde in complex real samples is difficult owing to its high volatility and reactivity. In this work, phenyl group-functionalized magnetic mesoporous microspheres were developed as the solid-phase extraction sorbents for enrichment and analysis of acetaldehyde in mainstream cigarette smoke. The functional magnetic microspheres were first synthesized through a facile one-pot co-condensation approach. The prepared nanomaterials possessed abundant silanol groups in the exterior surface and numerous phenyl groups in the interior pore-walls, as well as a large surface area (273.5 m 2 /g), strong superparamagnetism and uniform mesopores (3.3 nm). Acetaldehyde in mainstream cigarette smoke was collected in water and derivatizated with O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine. The formed acetaldehyde oximes were extracted and enriched by the prepared adsorbents via π–π interactions and subsequently analyzed using GC–MS. Extraction conditions such as amounts of sorbents, eluting solvent, adsorption and desorption time were investigated and optimized to achieve the best efficiency. Method validations including linearity, recovery, repeatability, and limit of detection were also studied. It was found that the suggested methodology provided low detection limit of 0.04 mg/mL, good recovery of 88–92%, intra-day and inter-day RSD values of 4.5% and 10.1%, and linear range of 0.25–4 mg/mL ( R 2 =0.999). The results indicated that the proposed method based on phenyl-functionalized magnetic mesoporous microspheres was rapid, efficient and convenient for the enrichment and analysis of acetaldehyde in tobacco.

A new one-step derivatization and microextraction technique was developed for determination of amino acids in tobacco samples. In the proposed method, amino acids were derivatized with isobutyl chloroformate (IBCF) in aqueous solution. The derivatives were extracted by dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME-SFO). Parameters affecting the extraction efficiency were investigated in detail. The optimum conditions were as follows: a mixture of 500 μL acetone, containing 40 μL 2-dodecanol, was rapidly injected by syringe into the 2 mL water sample. After centrifugation, the 2-dodecanol droplets were floated at the top of the tube. Then, the tube was cooled in an ice bath. After 5 min the solvent had solidified and was then transferred into a conical vial; it melted quickly at room temperature and it was injected into a gas chromatograph for analysis. Under the optimum conditions, the limits of detection were of the order of 0.12–2.82 μg/mL. The calibration curves showed good linearity over the investigated concentration range between 0.5 and 200 μg/mL with a coefficient of estimation (R2) > 0.9887 for GC–MS (SIM). The proposed method is an alternative approach to the quantification of amino acids in tobacco samples.

In this work, for the first time, headspace (HS) single-drop microextraction and simultaneous derivatization followed by GC-MS was developed to determine the aliphatic amines in tobacco samples. In the HS extraction procedure, the mixture of derivatization reagent and organic solvent was employed as the extraction solvent for HS single-drop microextraction and in situ derivatization of aliphatic amine in the samples. Fast extraction and simultaneous derivatization of the analytes were performed in a single step, and the obtained derivatives in the microdrop extraction solvent were analyzed by GC-MS. The optimized experiment conditions were: sample preparation temperature of 80 degrees C and time of 30 min, HS extraction solvent (the mixture of benzyl alcohol and 2,3,4,5,6-pentafluorobenzaldehyde) volume of 2.0 microL, extraction time of 90 s. With the optimal conditions, the method validations were also studied. The method has good linearity (R(2) more than 0.99), accepted precision (RSD less than 13%), good recovery (98-104%) and low limit of detection (0.11-0.97 microg/g). Finally, the proposed technique was successfully applied to the analyses of aliphatic amines in tobacco samples of seven different brands. It was further demonstrated that the proposed method offered a simple, low-cost and reliable approach to determine aliphatic amines in tobacco samples.

In this work, the novel technique based on headspace single-drop microextraction with in-syringe derivatization followed by GC-MS was established to determine the volatile organic acids in tobacco. The parameters for headspace single-drop microextraction and in-syringe derivatization were optimized, including extraction time, and volume of derivatization reagent and in-syringe derivatization time. The method validations including linearity, precision, recovery and LOD were also studied. The obtained results illustrated that the optimized technique was easy, highly efficient and sensitive. Finally, the proposed method was successfully applied to the analyses of volatile organic acids in tobacco samples with seven different brands. It was further demonstrated that the present technique developed in this study does offer a simple and fast approach to determine volatile organic acids in tobacco.

Flos Chrysanthemi Indici is a common traditional Chinese medicine (TCM). In this paper, headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS-SPME-GC-MS) was developed for quality assessment of Flos Chrysanthemi Indici from different growing areas in China. SPME parameters such as extraction fibers, extraction temperature, extraction time and sample mass were investigated to achieve identical results to those obtained by the steam distillation (SD). The selected SPME conditions were as follows: SPME fiber coated with 65-microm PDMS/DVB, extraction temperature of 60 degrees C, extraction time of 30 min and sample mass of 1.0 g. Furthermore, four active compounds (eucalyptol, camphor, borneol and bornyl acetate) presented in the TCM were applied to evaluating the quality of Flos Chrysanthemi Indici from 20 various areas. The quality assessment was successfully performed to compare the similarity value (S) between different sample vector of Flos Chrysanthemi Indici and the standard profile vector (SPV). The results showed that the proposed HS-SPME-GC-MS was an alternative technique for quality assessment of Flos Chrysanthemi Indici samples.

Crotonaldehyde has long been regarded as an important environmental pollutant from cigarette smoke to human health. To have an efficient and high-throughput screening of crotonaldehyde in saliva samples, it is essential to develop an analytical method considering both enrichment and measurement processes. In this study, we proposed a novel method based on matrix assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) for the analysis of crotonaldehyde in saliva. Magnetic graphene was synthesized via a facile hydrothermal process, and then applied as an adsorbent and a matrix for MALDI-TOF-MS. Crotonaldehyde in saliva was derived by 2,4-dinitrophenylhydrazine first followed by a magnetic solid-phase extraction process and high-throughput MALDI-TOF-MS detection. Due to its large surface area, strong interaction force and excellent inherent properties, magnetic graphene showed a satisfactory ionization and enrichment performance for the enrichment and ionization of crotonaldehyde by MALDI-TOF-MS. The crotonaldehyde derivatives could be sensitively detected from saliva samples even at a low concentrations. The results indicated that the proposed method was simple, rapid, sensitive and efficient for the analysis of crotonaldehyde in saliva and other biological samples.

Phenol is a mainstream cigarette smoke constituent and has been classified as a main toxic component directly related to environmental and health issues. Analysis of phenol in mainstream cigarette smoke is of great importance. In this work, microwave-assisted headspace solid-phase microextraction (HS-SPME) was developed for the fast analysis of phenol in a cigarette pad. Analyte in a Cambridge cigarette pad, activated by a short period of microwave irradiation, was headspace extracted by SPME and analyzed by GC-MS. Extraction conditions such as microwave irradiation time, SPME fiber coating, adsorption time and desorption time were investigated and optimized to achieve the best effect. The method was validated through the investigation of linearity, detection limit, recovery and precision. The linearity was in a wide range of 0.005–1 μg mL−1 with a correlation coefficient R2 = 0.999. The limit of detection was as low as 0.5 ng mL−1, and acceptable recovery and RSD values of 86.5% and 11.5% were achieved. The proposed method was successfully applied to the analysis of phenol in cigarette pad samples. The experimental results have demonstrated that microwave-assisted HS-SPME followed by GC-MS was a rapid, efficient and convenient method for the determination of phenol in tobacco products.