A Full Evaporation Static Headspace Gas Chromatography Method with Nitrogen Phosphorous Detection for Ultrasensitive Analysis of Semi-volatile Nitrosamines in Pharmaceutical Products

The recent detection of potent carcinogenic nitrosamine impurities in several human medicines has triggered product recalls and interrupted the supply of critical medications for hundreds of millions of patients, illuminating the need for increased testing of nitrosamines in pharmaceutical products. However, the development of analytical methods for nitrosamine detection is challenging due to high sensitivity requirements, complex matrices, and the large number and variety of samples requiring testing. Herein, we report an analytical method for the analysis of a common nitrosamine, N-nitrosodimethylamine (NDMA), in pharmaceutical products using full evaporation static headspace gas chromatography with nitrogen phosphorous detection (FE-SHSGC-NPD). This method is sensitive, specific, accurate, and precise and has the potential to serve as a universal method for testing all semi-volatile nitrosamines across different drug products. Through elimination of the detrimental headspace-liquid partition, a quantitation limit of 0.25 ppb is achieved for NDMA, a significant improvement upon traditional LC-MS methods. The extraction of nitrosamines directly from solid sample not only simplifies the sample preparation procedure but also enables the method to be used for different products as is or with minor modifications, as demonstrated by the analysis of NDMA in 10+ pharmaceutical products. The in situ nitrosation that is commonly observed in GC methods for nitrosamine analysis was completely inhibited by the addition of a small volume solvent containing pyrogallol, phosphoric acid, and isopropanol. Employing simple procedures and low-cost instrumentation, this method can be implemented in any analytical laboratory for routine nitrosamine analysis, ensuring patient safety and uninterrupted supply of critical medications.

Brewing on an industrial and a craft scale – impact on the physicochemical properties and volatile compounds profile of the pale pilsener-style lager beer analysed with HS/GC-MS

The pale Pilsener-style lager beers produced on a massive and craft scale were taken to analyse their basic physicochemical properties (alcohol content, pH, haze, real degree of fermentation) and volatile compounds profiles. The research was carried out using a beer analyser equipment and a headspace gas chromatography-mass spectrometry method (HS/GC-MS). The findings showed that in terms of physicochemical and flavour attributes, the quality of craft beers differed to a higher degree from the standard Pilsener beer quality than in the case of industrial beers.

Comparative Analysis and Development of a Flavor Fingerprint for Volatile Compounds of Vegetable Soybean Seeds Based on Headspace-Gas Chromatography-Ion Mobility Spectrometry

Evaluating the volatile compounds and characteristic fingerprints of the core cultivars of vegetable soybean would provide useful data for improving their aroma in the breeding programs. The present study used headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS) to evaluate the volatile compounds of vegetable soybean seeds at a specific growth stage. In total, 93 signal peaks were identified, 63 compounds qualitatively, with 14 volatile flavor compounds providing multiple signals. The 63 volatile compounds consisted of 15 esters, 15 aldehydes, 13 alcohols, 15 ketones, one acid, and four other compounds. The peak intensity of most of the volatile compounds varied greatly between the core cultivars. The alcohols and aldehydes determined the basic volatile flavor of the vegetable soybean seeds. Volatile flavors were determined by their respective esters, ketones, or other components. Characteristic fingerprints were found in some core vegetable soybean cultivars. Four cultivars (Xiangdou, ZHE1754, Zhexian 65018-33, and Qvxian No. 1) had pleasant aromas, because of their higher content of 2-acetyl-1-pyrroline (2-AP). A principal component analysis (PCA) was used to distinguish the samples based on the signal intensity of their volatile components. The results showed that the composition and concentration of volatile compounds differed greatly between the core cultivars, with the volatile flavor compounds of soybeans being determined by the ecotype of the cultivar, the direction of breeding selection, and their geographical origin. Characteristic fingerprints of the cultivars were established by HS-GC-IMS, enabling them to be used to describe and distinguish cultivars and their offspring in future breeding studies.

UV-C Treatment Maintains the Sensory Quality, Antioxidant Activity and Flavor of Pepino Fruit during Postharvest Storage

This study examines ultraviolet-C (UV-C) treatment supplementation as a means of inhibiting the senescence of pepino fruit after harvest. Pepino fruits were subjected to 1.5 kJ/m2 UV-C treatments and then packed and stored at 10 °C for 28 d. Results showed that 1.5 kJ/m2 UV-C treatment had the greatest ability to maintain firmness, and reduced the level of respiration and ethylene production. Further analysis indicated that the 1.5 kJ/m2 UV-C treatment maintained the content of total soluble solids (TSS), chlorophyll, vitamin C, flavonoids, and total phenolics. Lower levels of malondialdehyde (MDA) and higher levels of antioxidant enzyme activity were found in UV-C treated fruit during storage. An electronic nose (E-nose) and headspace-gas chromatography-mass spectrometry (HS-GC-MS) was used to determine volatile compounds. Results revealed that the UV-C treatment may promote the synthesis of a large number of alcohols and esters by maintaining the overall level of acids, aldehydes, and esters in fruits. This may contribute to the maintenance of the flavor of harvested fruits. In conclusion, 1.5 kJ/m2 UV-C treatment was demonstrated to be an effective treatment for the maintenance of the sensory, nutritional, and flavor parameters of pepino fruit.

Changes of Volatile Flavor Compounds in Large Yellow Croaker (Larimichthys crocea) during Storage, as Evaluated by Headspace Gas Chromatography–Ion Mobility Spectrometry and Principal Component Analysis

The large yellow croaker is one of the most economically important fish in Zhoushan, Zhejiang Province, and is well known for its high protein and fat contents, fresh and tender meat, and soft taste. However, the mechanisms involved in its flavor changes during storage have yet to be revealed, although lipid oxidation has been considered to be one important process in determining such changes. Thus, to explore the changes in the flavor of large yellow croaker fish meat during different storage periods, the main physical and chemical characteristics of the fish meat, including the acid value, peroxide value, p-anisidine value, conjugated diene value, and identities of the various flavor substances, were investigated and analyzed by multivariable methods, including headspace gas chromatography–ion mobility spectrometry (GC-IMS) and principal component analysis (PCA). It was found that after 60 d storage, the types and contents of the aldehyde and ketone aroma components increased significantly, while after 120 d, the contents of ketones (2-butanone), alcohols (1-propanethiol), and aldehydes (n-nonanal) decreased significantly. More specifically, aldehyde components dominated over ketones and lipids, while the n-nonanal content showed a downward trend during storage, and the 3-methylbutanol (trimer), 3-methylbutanol (dimer, D), 3-pentanone (D), and 3-pentanone (monomer) contents increased, whereas these compounds were identified as the key components affecting the fish meat flavor. Furthermore, after 120 d storage, the number of different flavor components reached its highest value, thereby confirming that the storage time influences the flavor of large yellow croaker fish. In this context, it should be noted that many of these compounds form through the Maillard reaction to accelerate the deterioration of fish meat. It was also found that after storage for 120 d, the physical indices of large yellow croaker meat showed significant changes, and its physicochemical properties varied. These results therefore demonstrate that a combination of GC-IMS and PCA can be used to identify the differences in flavor components present in fish meat during storage. Our study provides useful knowledge for understanding the different flavors associated with fish meat products during and following storage.

Characteristic Volatile Fingerprints of Four Chrysanthemum Teas Determined by HS-GC-IMS

Volatile composition is an important feature that determines flavor, which actively affects the overall evaluation of chrysanthemum tea. In this study, HS-GC-IMS (headspace-gas chromatography-ion mobility spectrometry) was performed to characterize the volatile profiles of different chrysanthemum tea subtypes. Forty-seven volatiles of diverse chemical nature were identified and quantified. Partial least squares discriminant analysis (PLS-DA) revealed that four chrysanthemum teas were distinct from each other based on their volatile compounds. Furthermore, this work provides reference methods for detecting novel volatile organic compounds in chrysanthemum tea plants and products.