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Abstract This paper describes a case of medicine in disguise: seized tattoo inks containing lidocaine and tetracaine at high concentration. Identification of anaesthetics was performed by LC MS Q-TOF with ESI+ source, by accurate mass measurement and by comparing the fragmentation patterns of molecular ions, at 30 V and 10 V of collision-offset voltage, with reference standards. Quantification was also performed by LC MS Q-TOF on the chromatographic peaks in the extracted ion chromatograms, by calibration curves obtained at different standard concentrations and by standard additions approach. The measurement uncertainty was estimated from validation data. The paper gives also chromatographic parameters, MS and MS/MS data and a quantitation method, with a full validation, of other six "caines". Thus the paper intends to provide a tool for identification and quantitation of the most common local anaesthetics that could be fraudulently added to tattoo inks. The results here reported show that the seized samples of inks represent a serious health risk owing to the high anaesthetic content – therapeutic-like dosage – found. Graphical abstract A case of medicines in disguise is described: tattoo inks containing local anaesthetics. The paper reports the identification and quantification of lidocaine and tetracaine in tattoo inks samples. A MS and MS/MS Q-TOF method for identification and quantitation of eight caines in tattoo inks was validated. fx1 Highlights • A new case of medicine in disguise: seized tattoo inks containing local anaesthetics. • Identification and quantification of lidocaine and tetracaine by LC MS Q-TOF. • A mass spectrometric method for identification and quantitation of eight "caines" in tattoo inks. • High therapeutic dosages anaesthetics in tattoo inks: a risk for health. [ABSTRACT FROM AUTHOR]

Graphical abstract Highlights • A method to identify and quantify Histamine contamination in Gentamicin medicinal products and active pharmaceutical ingredients by QTOF LC/MS. • Hydrophilic interaction liquid chromatography (HILIC) allowed a perfect separation of Histamine from Gentamicin and preservatives. • High resolution Q-TOF mass spectrometry resulted in the best choice to solve a case of Histamine contamination. • A detailed description of method validation and measurement uncertainty evaluation was presented. Abstract Adverse reactions have been reported for antibiotics produced via fermentation with fish peptone due to Histamine contamination. Just few micrograms of Histamine can result in adverse reactions when administered intravenously. Thus in this paper a new method for identification and quantitation of Histamine at ppm levels in the antibiotic Gentamicin is described. The method is based on separation of Histamine from Gentamicin and other excipients present in the drug matrix, by hydrophilic interaction liquid chromatography (HILIC) coupled to a Q-TOF/MS detector; quantitation is based on the standard addition approach. The method was validated for repeatability, inter-day precision, specificity, accuracy (relative and absolute bias) linearity, limit of detection and quantitation. Uncertainty was estimated and evaluated by comparison with values expected according to the Horwitz theory. The method showed satisfactory performances and good sensitivity, reaching a limit of quantitation of approximately 1 ppm. The method proposed can be a starting point for the development of Histamine quantitation methods in other antibiotics or even in other medicinal products which active ingredient is produced via fermentation in presence of fish peptone. [ABSTRACT FROM AUTHOR]

A nontargeted approach based on liquid chromatography equipped with a quadrupole time-of-flight mass detector ( LC- MS Q- TOF) joined to nuclear magnetic resonance ( NMR) analysis allowed rapid identification and quantification of the anti-inflammatory drug aceclofenac in illegal Adderall tablets. The largest chromatographic peak had m/z = 354.030 and m/z = 376.012 matching, respectively, the ionic structures (M + H)+ and (M + Na)+ of a molecule M. The accurate mass data generated the molecular formula C16H13Cl2 NO4. A screening of the pharmaceutical active substances having that molecular formula together with the MS/ MS fragmentation pattern suggested aceclofenac. Aceclofenac structure was unambiguously confirmed by 1H and 13C NMR experiments. The aceclofenac content was 90 mg/tablet ( RSD 2%) as detected by quantitative NMR. Information on the identity and content of illegal drugs is required for legal purposes; it supports in evaluating the effective impact on users safety, and it is useful for control laboratories using a targeted approach in their analytical activities. [ABSTRACT FROM AUTHOR]

The effects of hydroxyl radical attack on a peptidic drug were studied in vitro. Different chemico-physical techniques were used to investigate structural damage induced by oxidative stress conditions in salmon calcitonin (sCT), a peptide hormone used in treating osteoporosis. Reversed-phase liquid chromatography (RP-HPLC), circular dichroism (CD) and transmission electron microscopy (TEM) were applied to measure formation of oxidation/degradation products and to reveal the conformational and ultrastructural modifications in the presence of OH· free radicals. Hydroxyl radicals were obtained from ferrous sulfate and ascorbic acid mixtures. The RP-HPLC results revealed the formation of new chromatographic peaks indicating a number of degradation/oxidation products formed in the presence of OH· free radicals. CD spectra showed slight protein conformational modifications as well as aggregation. TEM confirmed sCT aggregation and suggested the formation of fibrillar aggregates. [Copyright &y& Elsevier]