Pharmaceuticals constitute one of the most important emerging classes of environmental pollutants. A three‐phase solvent system of water, water containing 0.1% of formic acid and acetonitrile was successfully used to separate, by liquid chromatography with mass spectrometry (LC‐MS), polarity‐matched pharmaceuticals, that is, carbamazepine, clarithromycin, and erythromycin, as well as amoxicillin and metformin. Despite of polarity similarities, these pharmaceuticals were completely resolved in the analytical run time of 15 min. The optimized three‐phase solvent system based‐method was validated for the simultaneous analysis of six matched‐polarity pharmaceuticals in wastewater samples. Good linearity (coefficient of determination more than 0.993) and precision (relative standard deviation less than 15.66%) were achieved. Recovery of analytes from the wastewater was between 0.70 and 1.18. Limits of detections ranged from 0.0001 to 0.5114 µg/L. No significant matrix effect, evaluated by post extraction addition, was observed in the electrospray ionization (ESI) source. Then, this methodology has been successfully applied to environmental study of pharmaceutical residues occurring in influent and effluent wastewater samples, from the main wastewater treatment plant in Potenza (Basilicata, Southern Italy).
Apples represent a greater proportion of the worldwide fruit supply, due to their availability on the market and to the high number of existing cultivar varieties and apple-based products (fresh fruit, fruit juice, cider and crushed apples). Several studies on apple fruit metabolites are available, with most of them focusing on their healthy properties’ evaluation. In general, the metabolic profile of apple fruits strongly correlates with most of their peculiar characteristics, such as taste, flavor and color. At the same time, many bioactive molecules could be identified as markers of a specific apple variety. Therefore, a complete description of the analytical protocols commonly used for apple metabolites’ characterization and quantification could be useful for researchers involved in the identification of new phytochemical compounds from different apple varieties. This review describes the analytical methods published in the last ten years, in order to analyze the most important primary and secondary metabolites of Malus domestica fruits. In detail, this review gives an account of the spectrophotometric, chromatographic and mass spectrometric methods. A discussion on the quantitative and qualitative analytical shortcomings for the identification of sugars, fatty acids, polyphenols, organic acids, carotenoids and terpenes found in apple fruits is reported.
Nitrate and nitrite as sodium or potassium salts are usually added to meat products to develop the characteristic flavor, to inhibit the growth of microorganisms (particularly Clostridium botulinum), and effectively control rancidity by inhibiting lipid oxidation. However, both nitrate and nitrite ions need to be monitored for ensuring the quality and safety of cured meats. In this work, for the first time the content of nitrite and nitrate ions in homogenized meat samples of baby foods was determined by a validated method based on ion chromatography (IC) coupled with conductivity detection. Recoveries of nitrate and nitrite ions in meat samples were not lower than 84 ± 6%. The detection limits of nitrate and nitrite were 0.08 mg L−1 and 0.13 mg L−1, respectively. Five commercial samples of homogenized meat, namely lamb, rabbit, chicken, veal, and beef, for infant feeding were investigated; while nitrite content was below the detection limit, nitrate ranged from 10.7 to 21.0 mg kg−1. The results indicated that nitrate contents were below the European (EU) fixed value of 200 mg kg−1, and an acceptable daily intake of 3.7 mg kg−1 was estimated.
Rationale
The anionic surfactants, among which are alkyl ether sulfates (AESs), are the most used class of surfactants in cleansing applications. The negatively charged head group of AESs is a sulfate moiety linked with a variable number of ethylene oxide units, i.e. a polyethylene glycol chain. The hydrophobic part of an AES is constituted by a linear alkyl chain of carbon atoms, generally obtained from natural fatty acids. Coconut oil fatty acids, including the sodium salts of coceth sulfate (CES) with chemical formula CxHy (OCH2CH2)nOSO3Na, are widely used as feedstock for AESs synthesis. CES is added to many cleaning products and detergents defined as non‐aggressive. Currently, no detailed structural information concerning the alkyl chain length x and, more importantly, the degree of ethoxylation n has been reported.
Methods
A commercial standard solution of CES was characterized by tandem mass spectrometry, employing direct injection into the electrospray ionization (ESI) source of a a linear quadrupole ion trap mass spectrometer.
Results
Two series of oligomeric species, characterized by a C12 and C14 alkyl chains, i.e. [C12H25(OCH2CH2)nOSO3]− and [C14H29(OCH2CH2)nOSO3]− with n ranging from 0 to 7, were successfully identified. The interpretation of these data was very useful for CES identification in three commercial dishwasher cleaning products.
Conclusions
Direct injection MS/MS analysis of CES revealed a well‐defined molecular weight distribution and allowed the alkyl chain composition and the number of ethylene oxide units to be to identified.
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