Combinative effect of pulsed-light irradiation and solid-state fermentation on ginkgolic acids, ginkgols, ginkgolides, bilobalide, flavonoids, product quality and sensory assessment of Ginkgo biloba dark tea.

Pulsed light (PL) is a prospective non-thermal technology that can improve the degradation of ginkgolic acid (GA) and retain the main bioactive compounds in Ginkgo biloba leaves (GBL). However, only using PL hasn't yet achieved the ideal effect of reducing GA. Fermentation of GBL to make ginkgo dark tea (GDT) could decrease GA. Because different microbial strains are used for fermentation, their metabolites and product quality might differ. However, there is no research on the combinative effect of PL irradiation fixation and microbial strain fermentation on main bioactive compounds and sensory assessment of GDT. In this research, first, Bacillus subtilis and Saccharomyces cerevisiae were selected as fermentation strains that can reduce GA from the five microbial strains. Next, the fresh GBL was irradiated by PL for 200 s (fluences of 0.52 J/cm2), followed by B. subtilis, S. cerevisiae, or natural fermentation to make GDT. The results showed that compared with the control (unirradiated and unfermented GBL) and the only PL irradiated GBL, the GA in GDT using PL + B. subtilis fermentation was the lowest, decreasing by 29.74%; PL + natural fermentation reduced by 24.53%. The total flavonoid content increased by 14.64% in GDT using PL + B. subtilis fermentation, whose phenolic and antioxidant levels also increased significantly. Sensory evaluation showed that the color, aroma, and taste of the tea infusion of PL + B. subtilis fermentation had the highest scores. In conclusion, the combined PL irradiation and solid-state fermentation using B. subtilis can effectively reduce GA and increase the main bioactive compounds, thus providing a new technological approach for GDT with lower GA.

Overall Content of Salicylic Acid and Salicylates in Food Available on the European Market.

The study aimed to determine the salicylates content in 112 products available on the European market. Quantitative determination of free and conjugated forms of salicylic acid in food was performed using reversed-phase high-performance liquid chromatography with fluorescence detection. The salicylates contents ranged from 0 to 1675.79 (µg/100 g). The results of this study confirm the presence of salicylates in food products, as well as a broad content diversity of these compounds depending on the species, variety, and method of processing the food items. The results can be very helpful for nutritionists and dieticians in planning low-salicylates or high-salicylates diets.

Concurrent supercritical fluid chromatographic analysis of terpene lactones and ginkgolic acids in Ginkgo biloba extracts and dietary supplements.

Supercritical fluid chromatography was used to resolve and determine ginkgolic acids (GAs) and terpene lactones concurrently in ginkgo plant materials and commercial dietary supplements. Analysis of GAs (C13:0, C15:0, C15:1, and C17:1) was carried out by ESI (-) mass detection. The ESI (-) spectra of GAs simply displayed only the [M-H](-) pseudo-molecular ions, and selected ion monitoring (SIM) for those ions was used for the quantification. Analysis of terpene lactones (ginkgolides A, B, C, J and bilobalide) was complicated by in-source collision-induced dissociation (IS-CID) in the ESI source. Thus, MS analysis could be influenced by the fragmentation pattern produced by the IS-CID. However, it was established that the fragmentation pattern, measured by ion survival yield (ISY), was independent of analyte concentration or matrix at a fixed cone voltage in the ESI source. Therefore, MS with SIM mode was applicable for the analysis of these analytes. The reported method provided consistent and sensitive analysis for the analytes of interest. The LOQs and LODs were determined to be below 100 and 40 ng/mL for GAs and 1 µg/mL and 400 ng/mL for terpene lactones, respectively. Intra- and inter-day precisions were found to be satisfactory with RSDs being below 5.2 %. Analyte recoveries ranged from 87 to 109 %. The developed method was successfully applied to the analysis of 11 ginkgo plant samples and 8 dietary supplements with an analysis time of less than 12 min.

Optimization of matrix solid-phase dispersion for the rapid determination of salicylate and benzophenone-type UV absorbing substances in marketed fish.

A simple and effective method for the rapid determination of five salicylate and benzophenone-type UV absorbing substances in marketed fish is described. The method involves the use of matrix solid-phase dispersion (MSPD) prior to their determination by on-line silylation gas chromatography tandem mass spectrometry (GC-MS/MS). The parameters that affect the extraction efficiency were optimized using a Box-Behnken design method. The optimal extraction conditions involved dispersing 0.5g of freeze-dried powdered fish with 1.0g of Florisil using a mortar and pestle. This blend was then transferred to a solid-phase extraction (SPE) cartridge containing 1.0g of octadecyl bonded silica (C18), as the clean-up co-sorbent. The target analytes were then eluted with 7mL of acetonitrile. The extract was derivatized on-line in the GC injection-port by reaction with a trimethylsilylating (TMS) reagent. The TMS-derivatives were then identified and quantitated by GC-MS/MS. The limits of quantitation (LOQs) were less than 0.1ng/g.

Simultaneous determination of the UV-filters benzyl salicylate, phenyl salicylate, octyl salicylate, homosalate, 3-(4-methylbenzylidene) camphor and 3-benzylidene camphor in human placental tissue by LC-MS/MS. Assessment of their in vitro endocrine activity.

UV-filters are widely used in many personal care products and cosmetics. Recent studies indicate that some organic UV-filters can accumulate in biota and act as endocrine disruptors, but there are few studies on the occurrence and fate of these compounds in humans. In the present work, a new liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to assess the presence of six UV-filters in current use (benzyl salicylate, phenyl salicylate, octyl salicylate, homosalate, 3-(4-methylbenzylidene) camphor, and 3-benzylidene camphor) in human placental tissue is proposed. The method involves the extraction of the analytes from the samples using ethyl acetate, followed by a clean-up step using centrifugation prior to their quantification by LC-MS/MS using an atmospheric pressure chemical ionization (APCI) interface. Bisphenol A-d16 was used as surrogate for the determination of benzyl salicylate, phenyl salicylate, octyl salicylate and homosalate in negative mode and benzophenone-d10, was used as surrogate for the determination of 3-(4-methylbenzylidene) camphor and 3-benzylidene camphor in positive mode. The found limits of detection ranged from 0.4 to 0.6ngg(-1) and the limits of quantification ranged from 1.3 to 2.0ngg(-1), while variability was under 13.7%. Recovery rates for spiked samples ranged from 97% to 104%. Moreover, the interactions of these compounds with the human estrogen receptor alpha (hERα) and androgen receptor (hAR), using two in vitro bioassays based on reporter gene expression and cell proliferation assessment, were also investigated. All tested compounds, except benzyl salicylate and octyl salicylate, showed estrogenic activity in the E-Screen bioassay whereas only homosalate and 3-(4-methylbenzylidene) camphor were potent hAR antagonists. Although free salicylate derivatives and free camphor derivatives were not detected in the human placenta samples analyzed, the observed estrogenic and anti-androgenic activities of some of these compounds support the analysis of their occurrence and their role as endocrine disrupters in humans.

Assessment of potential causes of falsely positive Mycobacterium tuberculosis breath test.

A suite of volatiles have previously been identified as specific markers of Mycobacterium tuberculosis metabolism in vitro. These markers - methyl phenylacetate, methyl p-anisate, methyl nicotinate, o-phenylanisole with the addition of methyl salicylate, may also be derived from other sources and confound development of a breath test for tuberculosis. To identify potential sources of these potential biomarkers food products, cosmetics, TB medication, environmental air and cigarette smoke were analysed for these markers using solid phase microextraction coupled with Gas Chromatography/Mass Spectrometry. Breath from healthy subjects, including smokers was also tested. Methyl salicylate was commonly detected, making this unsuitable as a specific marker for M. tuberculosis. Methyl nicotinate was detected repeatedly in cigarettes. Methyl phenylacetate was detected in 1.7% of healthy subjects and o-phenylanisole in just 1% of healthy breath indicating these may be more suitable for inclusion in the tuberculosis breath test due to their low "background" level. These results justify further clinical studies to further explore these markers as specific indicators of M. tuberculosis infection.

What happens if people start drinking mouthwash as surrogate alcohol? A quantitative risk assessment.

Mouthwash ingestion has been observed in settings of restricted availability to alcoholic beverages such as in hospitals, prisons or military establishments. The literature offers limited evidence that ingredients of mouthwash may have health effects above the effects of ethanol. This study provides a quantitative risk assessment based on analysis of 30 mouthwash samples. All investigated brands contained alcohol, most of them menthol (93%), eucalyptol (90%), benzoic acid (87%), methyl salicylate (67%), and thymol (30%). For low risk drinking scenarios with average levels, only ethanol will exceed acceptable daily intakes (ADI). In worst case scenarios for alcohol dependent consumers ingesting 100g ethanol per day in the form of mouthwash, methyl salicylate will also exceeded the ADI by a factor of 17. The margin of exposure (MOE) for methyl salicylate, benzoates and thymol was below 100 for average scenarios, and below 10 for worst case scenarios, but ethanol is still the most toxic ingredient with MOE below 1. The occasional or even chronic ingestion of mouthwash may not cause health effects except the effects of ethanol alone. Only in extreme exposures, ingredients such as thymol or methyl salicylate could exacerbate the effects of ethanol, especially by contributing to metabolic acidosis.

UHPLC-ESI/TOFMS determination of salicylate-like phenolic gycosides in Populus tremula leaves.

Associations of salicylate-like phenolic glycosides (PGs) with biological activity have been reported in Salix and Populus trees, but only for a few compounds, and in relation to a limited number of herbivores. By considering the full diversity of PGs, we may improve our ability to recognize genotypes or chemotype groups and enhance our understanding of their ecological function. Here, we present a fast and efficient general method for salicylate determination in leaves of Eurasian aspen that uses ultra-high performance liquid chromatography-electrospray ionization/time-of-flight mass spectrometry (UHPLC-ESI/TOFMS). The time required for the liquid chromatography separations was 13.5 min per sample, compared to around 60 min per sample for most HPLC protocols. In leaf samples from identical P. tremula genotypes with diverse propagation and treatment histories, we identified nine PGs. We found the compound-specific mass chromatograms to be more informative than the UV-visible chromatograms for compound identification and when quantitating samples with large variability in PG content. Signature compounds previously reported for P. tremoloides (tremulacin, tremuloidin, salicin, and salicortin) always were present, and five PGs (2'-O-cinnamoyl-salicortin, 2'-O-acetyl-salicortin, 2'-O-acetyl-salicin, acetyl-tremulacin, and salicyloyl-salicin) were detected for the first time in P. tremula. By using information about the formic acid adduct that appeared for PGs in the LTQ-Orbitrap MS environment, novel compounds like acetyl-tremulacin could be tentatively identified without the use of standards. The novel PGs were consistently either present in genotypes regardless of propagation and damage treatment or were not detectable. In some genotypes, concentrations of 2'-O-acetyl-salicortin and 2'-O-cinnamoyl-salicortin were similar to levels of biologically active PGs in other Salicaceous trees. Our study suggests that we may expect a wide variation in PG content in aspen populations which is of interest both for studies of interactions with herbivores and for mapping population structure.

Dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry for the rapid and sensitive determination of UV filters in environmental water samples.

The performance of the dispersive liquid-liquid microextraction (DLLME) technique for the determination of eight UV filters and a structurally related personal care species, benzyl salicylate (BzS), in environmental water samples is evaluated. After extraction, analytes were determined by gas chromatography combined with mass spectrometry detection (GC-MS). Parameters potentially affecting the performance of the sample preparation method (sample pH, ionic strength, type and volume of dispersant and extractant solvents) were systematically investigated using both multi- and univariant optimization strategies. Under final working conditions, analytes were extracted from 10 mL water samples by addition of 1 mL of acetone (dispersant) containing 60 µL of chlorobenzene (extractant), without modifying either the pH or the ionic strength of the sample. Limits of quantification (LOQs) between 2 and 14 ng L(-1), inter-day variability (evaluated with relative standard deviations, RSDs) from 9% to 14% and good linearity up to concentrations of 10,000 ng L(-1) were obtained. Moreover, the efficiency of the extraction was scarcely affected by the type of water sample. With the only exception of 2-ethylhexyl-p-dimethylaminobenzoate (EHPABA), compounds were found in environmental water samples at concentrations between 6 ± 1 ng L(-1) and 26 ± 2 ng mL(-1).

Personal decontamination after exposure to stimulated liquid phase contaminants: functional assessment of a new unit.

OBJECTIVE: To evaluate the efficacy of a decontamination station following exposure of volunteers to liquids with physical characteristics comparable to sarin and mustard gas. DESIGN: Twenty-four volunteers participated in the experiment which was performed with all staff wearing personal protective equipment including respiratory protection. The clothes, skin, and hair of the volunteers were contaminated with the simulated liquid phase contaminants, ethyl lactate and methyl salicylate. Sulphur hexafluoride gas was used to confirm the ventilation efficacy. Decontamination followed guidelines using a two-stage procedure. In the first chamber, all volunteers received a 3-minute shower with water at 30 degrees C, and their clothes but not their respiratory masks were removed. In the second, they were twice washed thoroughly with soap and water. After decontamination, the volunteers entered a third chamber for first aid measures. RESULTS: The air concentration of sulphur hexafluoride was reduced by 1:10,000 between the first and the third chambers. Ethyl lactate and methyl salicylate were measured in low concentrations in the third chamber. The capacity was 16 volunteers per hour with two-thirds on stretchers. After self-decontamination of the staff, the concentration of ethyl lactate increased significantly in the third chamber, consistent with residual ethyl lactate adsorbed by their underwear. This observation revealed a deficiency in the guidelines for self-decontamination. CONCLUSION: The capacity of the decontamination unit was found to be 16 volunteers per hour. The ventilation system and guidelines of the decontamination unit were demonstrated to be effective under the conditions examined. The self-decontamination of the staff was not optimal.

Assessment of triethanolamine salicylate release from the dermatological bases and the commercial products.

Recently, triethanolamine salicylate (TEAS) is frequently being incorporated in several over-the-counter topical analgesic pharmaceutical products. Since the clinical efficacy of such dosage form depends upon the release of the active ingredient at the site of application, the present study was undertaken to study the in vitro release of the (TEAS) from commonly used ointment bases and two most popular commercial products in the U.S. market. Also, the effects of various penetration enhancers, such as, ethanol, propylene glycol, polyethylene glycol-400, dimethyl-sulfoxide (DMSO), polysorbate-80 and urea were evaluated. In general, the drug release from the experimental formulations was higher than the commercial products studied. The inclusion of the penetration enhancing ingredients increased the drug release from some of the formulations evaluated. The hydrophilic emulsion base with 10% ethanol exhibited the best in vitro drug release. The apparent viscosity profiles of the formulations showed no definite relationship with the amounts of drug release. However, significant differences in the (TEAS) release from the experimental formulations were observed.