scholarly journals Simultaneous Determination of Acrylamide and Hydroxymethylfurfural in Extruded Products by LC-MS/MS Method

Molecules ◽  
2019 ◽  
Vol 24 (10) ◽  
pp. 1971 ◽  
Author(s):  
Antun Jozinović ◽  
Bojan Šarkanj ◽  
Đurđica Ačkar ◽  
Jelena Panak Balentić ◽  
Domagoj Šubarić ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Limit Of Detection ◽  
Raw Materials ◽  
Extrusion Process ◽  
Single Step ◽  
Liquid Chromatography Tandem Mass ◽  
Extruded Products ◽  
Snack Products ◽  
By Products

The aim of this study was to develop a liquid chromatography/tandem mass spectrometry LC-MS/MS method for the simultaneous determination of acrylamide and hydroxymethylfurfural (HMF) in corn snack products enriched with food industry by-products: brewer’s spent grain (BSG), sugar beet pulp (SBP) and apple pomace (AP). Development of the method included the study of different sources for ionization, different mobile phases, different extraction conditions as well as different methods of sample preparation. Finally, the single LC-MS/MS method was developed for the analysis of both analytes in one step with a duration of 20 min using a simple single-step extraction. The method with apparent recoveries of 91.4 and 90.4 for acrylamide and HMF, respectively, was applied for the analysis of non-extruded and extruded samples. The obtained results shown that the acrylamide content was <LOD (limit of detection) for all raw materials and non-extruded mixtures, while HMF increased proportionally to the content of added by-products in the mixtures. After the extrusion process, quantification of the acrylamide could be done in all samples. A higher amount of by-products entails higher contents of acrylamide and HMF, with the most significant effect in AP extrudates, where the highest content of HMF (6069 ± 789 ng/g) and acrylamide (5.37 ± 0.50 ng/g) in samples with 15% AP was observed.

scholarly journals Simultaneous Determination of Paracetamol, Chlorzoxazone, and Related Impurities 4-Aminophenol, 4'-Chloroacetanilide, and p-Chlorophenol in Pharmaceutical Preparations by High-Performance Liquid Chromatography

2007 ◽  
Vol 90 (1) ◽  
pp. 82-93 ◽  
Author(s):  
Mohammed Shahid Ali ◽  
Syed Rafiuddin ◽  
Mohsin Ghori ◽  
Aamer Roshanali Kahtri
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Limit Of Detection ◽  
Raw Materials ◽  
Pharmaceutical Preparations ◽  
Dosage Forms ◽  
Phase Detection ◽  
Constant Flow Rate ◽  
Related Impurities

Abstract This paper presents a simple, specific, and precise high-performance liquid chromatographic method for the simultaneous determination of paracetamol (PCM), chlorzoxazone (CXZ), and their related impurities in bulk raw materials and solid dosage forms. The mobile phase consisted of water methanolglacial acetic acid (60 + 40 2, v/v/v). A column containing octadecylsilane chemically bonded to porous silica particles (Spherisorb ODS 1, 25 cm × 4.6 mm, 5 μm) was used as stationary phase. Detection was performed using a variable wavelength ultraviolet-visible detector set at 272 nm for all compounds. Solutions were injected into the chromatograph under isocratic condition at a constant flow rate of 1.2 mL/min. The method was validated according to International Conference on Harmonization requirements and demonstrates good accuracy and precision and a wide linearity range. The method separates PCM, CXZ, and 3 major impurities 4-aminophenol (4AP), 4'-chloracetanilide (4CA), and p-chlorophenol (PCP) with fair resolution in less than 15 min. The developed method is rapid and sensitive (limit of detection for 4AP, 4CA, and PCP established at 31.25, 39.06, and 65.16 ng/mL, respectively) and, therefore, suitable for quality control and stability studies of these compounds in dosage forms.

scholarly journals Identification and Quantification of Enniatins and Beauvericin in Animal Feeds and Their Ingredients by LC-QTRAP/MS/MS

Metabolites ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 33 ◽  
Author(s):  
Josefa Tolosa ◽  
Yelko Rodríguez-Carrasco ◽  
Emilia Ferrer ◽  
Jordi Mañes
Keyword(s):  
Raw Materials ◽  
Mycotoxin Contamination ◽  
European Guidelines ◽  
Toxic Metabolites ◽  
Liquid Chromatography Tandem Mass ◽  
The Common ◽  
And Storage ◽  
Common Combination ◽  
By Products

Emerging fusariotoxins, mainly enniatins (ENNs) and beauvericin (BEA), are secondary toxic metabolites produced by Fusarium spp. and are widely distributed contaminants of cereals and by-products. Mycotoxin contamination in these products supposes an important risk to feed supply security in the feed industry due to the common use of cereals in feed formulations. Hence, continuous monitoring of both raw materials and feed mixtures is highly recommended as stated by sanitary authorities. Therefore, an analytical procedure based on liquid chromatography tandem mass spectrometry and an acetonitrile-based extraction followed by a d-SPE (QuEChERS) step for the simultaneous determination of emerging Fusarium mycotoxins was in-house validated and successfully applied to raw materials (n = 39) and feed manufactured with them (n = 48). The analytical method was validated following the European guidelines and satisfactory results were obtained. Both raw materials and complete feedstuffs showed mycotoxin contamination at incidences of 18% and 92%, respectively. ENN B was the most commonly found mycotoxin in the analyzed samples at concentrations up to several tens of µg/kg. On the other hand, the co-occurrence of mycotoxins was observed in 47% of samples, ENN B and BEA being the most common combination. These results highlight the necessity to take a vigilant attitude to monitor the occurrence of contaminants in raw materials and feedstuffs throughout the manufacturing chain and storage.

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