Identification of Key Odorants in Used Disposable Absorbent Incontinence Products.

PURPOSE: The purpose of this study was to identify key odorants in used disposable absorbent incontinence products. DESIGN: Descriptive in vitro study SUBJECTS AND SETTING:: Samples of used incontinence products were collected from 8 residents with urinary incontinence living in geriatric nursing homes in the Gothenburg area of Sweden. Products were chosen from a larger set of products that had previously been characterized by descriptive odor analysis. METHODS: Pieces of the used incontinence products were cut from the wet area, placed in glass bottles, and kept frozen until dynamic headspace sampling of volatile compounds was completed. Gas chromatography-olfactometry was used to identify which compounds contributed most to the odors in the samples. Compounds were identified by gas chromatography-mass spectrometry. RESULTS: Twenty-eight volatiles were found to be key odorants in the used incontinence products. Twenty-six were successfully identified. They belonged to the following classes of chemical compounds: aldehydes (6); amines (1); aromatics (3); isothiocyanates (1); heterocyclics (2); ketones (6); sulfur compounds (6); and terpenes (1). CONCLUSION: Nine of the 28 key odorants were considered to be of particular importance to the odor of the used incontinence products: 3-methylbutanal, trimethylamine, cresol, guaiacol, 4,5-dimethylthiazole-S-oxide, diacetyl, dimethyl trisulfide, 5-methylthio-4-penten-2-ol, and an unidentified compound.

A GC-ECD method for estimation of free and bound amino acids, gamma-aminobutyric acid, salicylic acid, and acetyl salicylic acid from Solanum lycopersicum (L.).

A gas chromatograph with electron capture detection method for estimation of selected metabolites--amino acids (free and bound), gamma-aminobutyric acid (GABA), salicylic acid (SA), and acetyl salicylic acid (ASA) from tomato--is reported. The method is based on nitrophenylation of the metabolites by 1-fluoro-2, 4-dinitrobenzene under aqueous alkaline conditions to form dinitophenyl derivatives. The derivatives were stable under the operating conditions of GC. Analysis of bound amino acids comprised perchloric acid precipitation of protein, alkylation (carboxymethylation) with iodoacetic acid, vapor-phase hydrolysis, and derivatization with 1-fluoro-2,4-dinitrobenzene in that order. The metabolites were resolved in 35 min, using a temperature-programmed run. The method is rapid, sensitive, and precise. It easily measured the typical amino acids (aspartate, asparagine, glutamate, glutamine, alanine, leucine, lysine, and phenylalanine) used for identification and quantification of a protein, resolved amino acids of the same mass (leucine and isoleucine), satisfactorily measured sulfur amino acid (methionine, cystine, and cysteine), and quantified GABA, SA, and ASA, as well. The developed method was validated for specificity, linearity, and precision. It has been applied and recommended for estimation of 25 metabolites from Solanum lycopersicum (L.).

Recent progress in food flavor analysis using gas chromatography-ion mobility spectrometry (GC-IMS).

Rapid, nondestructive, high-throughput testing and screening of volatile ingredients plays an important role in food flavor analysis. Gas chromatography-ion mobility spectrometry (GC-IMS) is a powerful technique for the separation and sensitive detection of volatile organic compounds. It has a fast response, high sensitivity, easy operation, and low cost. In this article, a brief introduction to the working principle of GC-IMS is presented. A summary of recent studies of different food flavor analysis applications is also provided, including food classification and adulteration, the evaluation of food freshness and spoilage, off-flavor detection, monitoring the processing of food products, and evaluation of aroma changes during food storage. Finally, future directions of GC-IMS are proposed.

Clinical reliability of non-organoleptic oral malodour measurements.

AIM: Measurement of volatile sulphur compounds (VSC) by portable sulphur monitors (Halimeter, OralChroma) is a common practice for diagnosis of oral malodour. In this study, the clinical value of these devices was examined. MATERIALS AND METHODS: Two hundred and eighty patients with bad breath complaints attending a halitosis consultation were enrolled. Organoleptic scores were given by a trained and calibrated judge, before measurement of the VSC levels (Halimeter, OralChroma), to avoid any bias. RESULTS: Significant correlations were found between the organoleptic assessment, the Halimeter, and the OralChroma (R=0.74 for organoleptic versus Halimeter; 0.66 for organoleptic versus OralChroma; 0.63 for Halimeterversus OralChroma). The sensitivity and specificity (with regard to the organoleptic score) to detect patients with/without oral malodour for the Halimeter were 63% and 98%, respectively, and for the OralChroma 69% and 100% when using the cutoffs suggested by the manufacturer. By lowering these values, sensitivity could be improved without a significant decrease in specificity (both devices). CONCLUSIONS: We concluded that the measurement of the VSC levels can be used as an adjunct to the organoleptic assessment. Thresholds should be revisited in order to improve their clinical utility. These devices can prove the absence of malodour in case of pseudo-halitosis.

Two metrics for measuring orthogonality for two-dimensional chromatography.

Orthogonality can be used as a selection parameter for two-dimensional chromatography column selection (e.g. in GC × GC or LC × LC) or for method optimization purposes, both aiming for maximal orthogonality for a particular analytical application. In order to improve the concurrence of two-dimensional chromatography expert's orthogonality grading, two orthogonality metrics, %FIT and %BIN, were developed, evaluated and compared with the Asterisks orthogonality metric. The %BIN is a bin counting approach where the number of bins is fixed at 25 and deviations from the expected average number of peaks per bin is used as the basis for the orthogonality calculation. The %FIT is based on fitting polynomials of degree two, through the xy and the yx data and calculating the average minimal distance and standard deviation of all data points above and below the fitted polynomials. The orthogonality metrics were evaluated by using 14 different types of computer generated xy datasets and two measured LC × LC datasets. Both %FIT and %BIN, were shown to have a larger discriminative power than the Asterisks equations, and are in good agreement with the orthogonality scores for 2D-chromatograms provided by nine experts.

Evaluation of the perceptual interaction among ester aroma compounds in cherry wines by GC-MS, GC-O, odor threshold and sensory analysis: An insight at the molecular level.

The ester aroma profiles of five Chinese cherry wines and the perceptual interaction among esters were investigated in this study. 24 esters were identified by Gas chromatography-olfactometry (GC-O) and Gas Chromatography-Mass Spectrometer (GC-MS). According to addition/omission analysis, seven volatile compounds among them were selected and studied using sensory profiling and multivariate statistic methods such as Principal Component Analysis (PCA). In sensory analysis, a significant reduction of olfactory threshold for total aromatic reconstitution was induced by the addition among each of them in Feller's additive model, which demonstrated their synergistic effects. The σ/τ plot showed that most of them were followed by a partial addition behavior. Furthermore, PCA indicated that the addition among each of them had a significant effect on fruity, floral, sweet and fermentation aroma intensity. Specifically, ethyl decanoate and methyl salicylate at sub-threshold concentrations were also likely to contribute to overall aroma. The results of perceptual interaction were mainly influenced by chemical structure and molecular polarity.

Inter-laboratory proficiency results of blood alcohol determinations at clinical and forensic laboratories in Italy.

BACKGROUND: Inter-laboratory proficiency schemes are widely used to control the performance of clinical and forensic toxicology laboratories. In 2016 the Laboratory of Environmental Hygiene and Forensic Toxicology - Venice (Italy) initiated an inter-laboratory proficiency test of blood-alcohol analysis. The number of participating laboratories gradually increased from 26 to 36. Furthermore, a few clinical laboratories were included if gas chromatographic (GC) methods were used for blood alcohol analysis. PROCEDURE: Whole blood was obtained from the Blood Transfusion Centre of the Venice Hospital and a mixture of sodium fluoride and potassium oxalate was added as a preservative and anticoagulant, respectively. Aliquots of the blood were spiked with certified pure ethanol to obtain target blood-alcohol concentrations (BACs) ranging from 0 to 5.0g/L. Two blood samples (4mL each) were included in each shipment to the participating laboratories. The laboratories were asked to provide information about number of replicate BAC determinations they made, the types of ethanol reference standards used, and inherent measurement uncertainty. The aim of the testing was to obtain a mean consensus value for the target BAC and to assess inter-laboratory imprecision. All procedures for registration and submission of results were done on-line. A confidential report and statistical evaluations were returned to the participants one week later. ANALYTICAL METHODS: All participants used head-space GC (HS-GC) for the analysis of ethanol in blood. More than 85% of participants used HS-GC with flame-ionization detection, whereas the others used mass spectrometry (MS) as a detector. More than 40% of the participating laboratories kept the blood samples frozen (-20°C) prior to analysis, whereas the others used refrigeration (+4°C). The preliminary validation tests showed that there were no statistically significant differences between BAC in frozen or refrigerated samples for a period of 20 days. RESULTS AND CONCLUSION: The statistical evaluation of results was done using an iterative procedure known as Algorithm A (ISO 13528:2015, C.3.1). This provides robust estimates for mean and standard deviation between laboratories and these were used as consensus values. More than 85% of participants provided satisfactory results (z-score <1) and 94% of laboratories were within z-score <2, based on five control samples. When a blood sample without any alcohol (blank) was sent for analysis, laboratories reported this as zero, 0.00g/L, below limit of detection (LOD) or not detected. Some type of consensus should be reached for reporting blank samples.

QSPR study on GC relative retention time of organic pesticides on different chromatographic columns.

In the present study, Lu index and distance-based atom type topological index (DAI) previously developed in our team, were introduced and combined with molecular electronegativity chi ep to characterize quantitative structure-property relationship of GC relative retention time (RRT) for several types of structurally diverse organic pesticides on the four kinds of chromatographic columns. Using multiple linear regression technique, four several-variable models are obtained with the estimations correlation coefficient (R(2)) being between 0.9655 and 0.9285, and the correlation coefficient (R(2)cv) in the leave-one-out cross-validation procedure are between 0.9560 and 0.9143, respectively. The results in this study indicate that the three topological indices Lu index, DAI, and molecular electronegativity chi ep can predict the gas chromatographic RRT of organic pesticides with diverse hetero-atoms.

An accurate and nondestructive GC method for determination of cocaine on US paper currency.

The presence of cocaine on US paper currency has been known for a long time. Banknotes become contaminated during the exchange, storage, and abuse of cocaine. The analysis of cocaine on various denominations of US banknotes in the general circulation can provide law enforcement circles and forensic epidemiologists objective and timely information on epidemiology of illicit drug use and on how to differentiate money contaminated in the general circulation from banknotes used in drug transaction. A simple, nondestructive, and accurate capillary gas chromatographic method has been developed for the determination of cocaine on various denominations of US banknotes in this study. The method comprises a fast ultrasonic extraction using water as a solvent followed by a SPE cleanup process with a C(18) cartridge and capillary GC separation, identification, and quantification. This nondestructive analytical method has been successfully applied to determine the cocaine contamination in US paper currency of all denominations. Standard calibration curve was linear over the concentration range from the LOQ (2.00 ng/mL) to 100 microg/mL and the RSD less than 2.0%. Cocaine was detected in 67% of the circulated banknotes collected in Southeastern Massachusetts in amounts ranging from approximately 2 ng to 49.4 microg per note. On average, $5, 10, 20, and 50 denominations contain higher amounts of cocaine than $1 and 100 denominations of US banknotes.

Determination of organotins in aquatic food by gas chromatography with pulsed flame photometric detection.

A method based on gas chromatography (GC)-pulsed flame photometric detection (PFPD) was developed to determine the levels of organotins in aquatic food. After being purified by gel-permeation chromatography in ethyl actate-tetrahydrofuran, the organotin compounds were derivatized by pentylmagnesium bromide. The derivative products were injected into the GC system and detected by PFPD (sulfur mode). The method was validated by analysis of the certified reference material and spiked samples. Recoveries of organotins ranged from 84.1 to 116.6% with relative standard deviation between 1.3 and 16.0% when spiked at levels of 2, 10, and 40 microg/kg. The limits of detection varied from 0.1 to 1.2 microg/kg for shellfish and 0.1 to 0.5 microg/kg for fish. The proposed method was suitable for determining organotins in aquatic foods.

Analysis of trace amounts of carbon dioxide, oxygen and carbon monoxide in nitrogen using dual capillary columns and a pulsed discharge helium ionisation detector.

Gas mixtures of trace amounts of carbon dioxide (CO(2)), dioxygen (O(2)), and carbon monoxide (CO) in dinitrogen (N(2)) were separated and quantified using parallel dual capillary columns and pulsed discharge helium ionisation detection (PDHID). The detection limits (9 x 10(-9) mol mol(-1) for CO(2), 7 x 10(-9) mol mol(-1) for O(2) and 37 x 10(-9) mol mol(-1) for CO) were lower than those reported previously for similar methods. Uncertainties were calculated and results were validated by comparison of the CO and CO(2) results with those obtained using conventional methods. The method was also used to analyse nitrogen, carbon dioxide and carbon monoxide in oxygen.

Quantitative structure and retention relationships for gas chromatographic data: application to alkyl pyridines on apolar and polar phases.

Quantitative structure and retention relationships (QSRR) have been developed to model gas chromatographic retention data of alkyl pyridines on apolar (branched alkane) and polar (primary alcohol) stationary phases. The retention properties analyzed are Kovats retention index, I; partial molar enthalpy, DeltaH; partial molar entropy, DeltaS and partition coefficient, log K. Using the seven valence molecular connectivity indices (chi) calculated for the 18 alkyl pyridines, regression models are generated to predict the retention properties. The best model (model A) obtained with the descriptors ((1)chi(P)(V), (3)chi(P)(V) and (6)chi(CH)(V) was unable to produce a satisfactory statistical performance and correct order of elution. The model has been modified (model B) by including steric parameter s, which has been empirically derived by considering the steric effects due to the presence of alkyl groups at the ortho and meta positions. The modified model predicts the correct order of elution for all the alkyl pyridines and good correlation coefficients, r. The r values obtained for I, DeltaH, DeltaS and log K are: r=0.955, 0.975, 0.984 and 0.955 (model A) become r=0.999, 0.996, 0.990 and 0.999 (model B) on the apolar stationary phase and r=0.931, 0.926, 0.911 and 0.931 (model A) become r=0.999, 0.992, 0.958 and 0.999 (model B) on the polar stationary phase.

Determination of eight synthetic pyrethroids in bovine fat by gas chromatography with electron capture detection.

Synthetic pyrethroids are among the most widely used classes of insecticides, and their uses are varied, including plant protection, animal dips, and as a treatment for human clothing and bedding in very hot climates. Veterinary applications include ear tags, pour-on formulations, sprays, and dips. Persistent residues have been reported in livestock, and routine monitoring programs in other countries have found detectable residues of various pyrethroids in fat. A method has been developed using solid-phase extraction that reduces the quantities of solvents used, the time required, and the amount of glassware used compared to an earlier method on which it was based. The scope of analytes tested included the 5 compounds cited in the earlier method (flucythrinate, permethrin, cypermethrin, fenvalerate, and deltamethrin) and, in addition, cyfluthrin, lambda-cyhalothrin, and fluvalinate. Sample extracts were analyzed by gas chromatography with electron capture detection using selected chromatographic peaks characteristic of each compound. Limits of quantification for the compounds were from 25-50 microg/kg, with a linear response for all compounds to 200 microg/kg. Recoveries ranged from 80 to 123%.

Simple automatic strategy for background drift correction in chromatographic data analysis.

Chromatographic background drift correction, which influences peak detection and time shift alignment results, is a critical stage in chromatographic data analysis. In this study, an automatic background drift correction methodology was developed. Local minimum values in a chromatogram were initially detected and organized as a new baseline vector. Iterative optimization was then employed to recognize outliers, which belong to the chromatographic peaks, in this vector, and update the outliers in the baseline until convergence. The optimized baseline vector was finally expanded into the original chromatogram, and linear interpolation was employed to estimate background drift in the chromatogram. The principle underlying the proposed method was confirmed using a complex gas chromatographic dataset. Finally, the proposed approach was applied to eliminate background drift in liquid chromatography quadrupole time-of-flight samples used in the metabolic study of Escherichia coli samples. The proposed method was comparable with three classical techniques: morphological weighted penalized least squares, moving window minimum value strategy and background drift correction by orthogonal subspace projection. The proposed method allows almost automatic implementation of background drift correction, which is convenient for practical use.

Paroxetine levels in postpartum depressed women, breast milk, and infant serum.

BACKGROUND: The purpose of this study was to determine the concentrations of paroxetine in maternal serum, breast milk, and infant serum samples and to estimate infant exposure through breastfeeding. METHOD: A total of 25 sample sets was obtained: I sample set each from 23 mother-infant dyads and 2 sample sets from 1 mother-infant dyad. All mothers met DSM-IV criteria for major depressive disorder. The maternal fixed dosage of paroxetine was 10, 20, or 40 mg/day for a minimum of 30 days before the samples were drawn. Samples were collected 6 hours after dose intake, and the concentration of paroxetine in each sample was determined using gas chromatography/mass spectrometry. The analytic method employed in this study is the most sensitive to date, with the ability to detect drug concentrations as low as 0.1 ng/mL. RESULTS: Detectable levels of paroxetine were present in all maternal serum samples and in 24 of the 25 breast milk samples. In all of the infant serum samples, the paroxetine concentrations were below the lower limit of quantification. No unusual adverse effects were reported in any of the infants. CONCLUSION: The results of this study demonstrate that paroxetine, like the other selective serotonin reuptake inhibitors studied to date, is excreted into the breast milk of nursing mothers. The mean infant dose of paroxetine was 1. 1% of the maternal dose. Although no short-term adverse effects were reported in any of the infants in this study, future studies are needed to address a more systematic method for observing and recording any adverse effects. In addition, future studies should incorporate follow-up studies in order to evaluate possible long-term effects of paroxetine exposure.

Application of a new method for analysis of exhaled gas in critically ill patients.

OBJECTIVE: Application of a new method for analysis of exhaled gas in critically ill patients. DESIGN: Open study. SETTING: Surgical intensive care unit of an university hospital. PATIENTS: Thirty-seven consecutive, critically ill, mechanically ventilated patients. INTERVENTIONS: None. MEASUREMENTS AND RESULTS: Chemical analysis of the patient's exhaled gas was based upon substance adsorption and concentration onto activated charcoal, microwave desorption and gas chromatographic separation. Patients with acute respiratory distress syndrome (ARDS) exhaled less isoprene than those without ARDS [9.8 (8.2-21.6) vs 21.8 (13.9-41.4) nmol/m2 per min [median (95% confidence interval)], p = 0.04]. In patients who developed pulmonary infection, pentane elimination increased from 0.4 (0.0-5.4) to 2.7 (0.6-6.1, p = 0.05) nmol/m2 per min and isoprene elimination decreased from 5.2 (0-33) to 5.0 (0-17, p = 0.05) nmol/m2 per min, resulting in a significant increase in pentane/isoprene ratio from 0.1 (0-0.3) to 0.4 (0-15, p = 0.007) when compared to patients without pulmonary infection. CONCLUSIONS: The new method allows quantitative analysis of human gas samples with low substance concentrations and is well suited for clinical studies which involve the investigation of metabolic processes in the lung and the body.

Limited sampling strategy to predict AUC of the CYP3A phenotyping probe midazolam in adults: application to various assay techniques.

Midazolam clearance is used to phenotype hepatic CYP3A activity but requires multiple plasma samples following a single intravenous dose. The authors evaluated the use of a limited sampling scheme, using different assay techniques to determine the reproducibility of such a strategy in estimating midazolam AUC. Seventy-three healthy adults received midazolam as a single intravenous bolus dose. At least eight plasma samples were collected from each subject and were assayed using either LC/MS/MS or electron capture gas chromatography. Eleven subjects were randomly selected for the training set using stepwise linear regression to determine relationships between midazolam plasma concentrations and AUC. Validation of the predictive equations was done using the remaining 62 subjects. Mean percent error (MPE), mean absolute error (MAE), and root mean square error (RMSE) were calculated to determine bias and precision. Based on the training set, five models were generated with coefficients of determination ranging from 0.87 to 0.95. Validation showed that MPE, MAE, and RMSE values were acceptable for three of the models. Intrasubject reproducibility was good. In addition, training set datafrom one institution were able to predict data from the other two institutions using other assay techniques. Minimized plasma sampling mayprovide a simpler method for estimating midazolam AUC for CYP3A phenotyping. A limited sampling strategy is more convenient and cost-effective than standard sampling strategies and is applicable to more than one assay technique.

Purge-and-trap method for the determination of styrene in urine.

A purge-and-trap method for biological monitoring of styrene in urine was developed. Sorbent tubes packed with Tenax TA were used to trap styrene vapour purged from urine. Thermal desorption-gas chromatography was used for sorbent tubes analysis. The detection limit (0.70 micrograms/1), linearity range, recovery (> 94% for spiked urine samples) and repeatability for urine from occupational exposed workers show the suitability of the method for the determination of styrene in urine. One specific advantage of this method is the possibility of storage of the charged sorbent tubes during long periods of time without a significant loss of styrene. This approach can be used, with slight modifications, for urinary determination of several others organic contaminants commonly present in occupational exposures.

Analysis of trichloroacetic acid in the urine of workers occupationally exposed to trichloroethylene by capillary gas chromatography.

A gas chromatographic procedure is described for the determination of trichloroacetic acid in urine, the major metabolite of trichloroethylene exposure. Trichloroacetic acid was derivatised to its methyl ester with BF3/methanol reagent and then extracted into toluene and analysed by capillary gas chromatography using electron-capture detection. The response was linear in the range 0.4-100 mg/l of trichloroacetic acid in urine and showed a relative recovery of 99.6%. The procedure is suitable for monitoring occupational exposure to trichloroethylene.

Automated solid-phase extraction coupled to gas chromatography with electron-capture detection: a combination of extraction and clean-up of pyrethroids in the analysis of surface water.

The combination of automated solid-phase extraction (SPE) and large-volume introduction gas chromatography electron-capture detection (GC-ECD) is used for the determination of synthetic pyrethroids in surface and drinking water. The selectivity that is needed for the use of GC-ECD of environmental samples is achieved by addition of a polarity modifier to the sample. In this study, sufficient methanol was added to 19 ml of sample to obtain a level of 30% of modifier prior to SPE. The cartridge is washed with one additional ml of 30% methanol in water. After drying, the cartridge is eluted with toluene. GC-ECD analysis is performed by on-column introduction of 100 microliters of the toluene extract. The whole procedure was automated by using an automated solid-phase extraction apparatus. Limits of detection (LODs) for the pyrethroids in surface water are in the range of 1 to 8 ng/1 (signal-to-noise ratio = 3); even lower limits of detection are possible for drinking water.