Development and validation of a solid-phase extraction and gas chromatography–tandem mass spectrometry method for the determination of isopropyl-9H-thioxanthen-9-one in carton packaged milk

Allegrone, Gianna; Tamaro, Ilaria; Spinardi, Shara; Grosa, Giorgio

doi:10.1016/j.chroma.2008.10.019

Cited by 29 publications

(16 citation statements)

References 7 publications

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“…A few methods based on LC in combination with UV detection (Papilloud et al 2002;Sanches-Silva et al 2008a, 2008b, 2009 or even fluorescence detection have also been reported (Morlock & Schwak 2006;Sagratini et al 2008). However, LC-MS/MS has gained popularity (Sagratini et al 2006;Bagnati et al 2007;Gil-Vergara et al 2007;Sun et al 2007;Allegrone et al 2008;Gallart-Ayala et al 2008, 2011Sanches-Silva et al 2008;Shen et al 2009). A comparison between GC and LC has shown, however, that both techniques are adequate: LC gives a lower LOQ while the repeatability is comparable (Gil-Vergara et al 2007).…”

Section: Introductionmentioning

confidence: 95%

Evaluation of the migration of 15 photo-initiators from cardboard packaging into Tenax^®using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

Houwe

Velde

Evrard

et al. 2014

Food Additives & Contaminants: Part A

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Photo-initiators are widely used to cure ink on packaging materials used in food applications such as plastic films or cartonboards. In migration studies, food simulants are very often used to simulate food, like Tenax(®), which is the simulant for dry foodstuffs. In this paper a fast and reliable confirmation method for the determination of the following photo-initiators in Tenax(®) is described: benzophenone (BP), 4,4'-bis(diethylamino)benzophenone (DEAB), 2-chloro-9H-thioxanthen-9-one (CTX), 1-chloro-4-propoxy-9H-thioxanthen-9-one (CPTX), 2,4-diethyl-9H-thioxanthen-9-one (DETX), 2,2-dimethoxy-2-phenyl acetophenone (DMPA), 4-(dimethylamino)benzophenone (DMBP), 2-ethylanthraquinone (EA), ethyl-4-dimethylaminobenzoate (EDMAB), 1-hydroxylcyclohexyl phenyl ketone (HCPK), 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone (HMMP), 2-isopropyl-9H-thioxanthen-9-one (ITX), 4-methylbenzophenone (MBP), Michler's ketone (MK), and 4-phenylbenzophenone (PBZ). After the migration study was completed, the simulant Tenax(®) was extracted using acetonitrile, followed by analysis on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Quantification was carried out using benzophenone-d10 (BP-d10) as internal standard. The presented method is validated in terms of matrix effect, specificity, linearity, recovery, precision and sensitivity, showing the method can detect all photo-initiators at very low concentrations (LOD < 0.125 µg g(-1) for all substances). Finally, the procedure was applied to real samples, proving the capabilities of the presented method.

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Section: Introductionmentioning

confidence: 95%

Evaluation of the migration of 15 photo-initiators from cardboard packaging into Tenax^®using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

Houwe

Velde

Evrard

et al. 2014

Food Additives & Contaminants: Part A

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“…As in liquid chromatography, different detectors can be used with this technique, and the mass detector is the most commonly used (GC-MS), 16,22,24,28,36,[44][45][46][47][48][49] although in this case the use of mass-mass tandem is not very common. 50 The chromatographic separation was achieved with a low polar capillary column: HP-5 (Agilent s ) ((5%-phenyl)-methylpolysiloxane) (i.d., 30 mÂ0.32 mm and film thickness, 0.25 mm). The system was operated in splitless mode, with the oven temperature programmed to increase from 100 to 300 1C, and the detector temperature was set at 250 1C.…”

Section: Gas Chromatography (Gc)mentioning

confidence: 99%

“…Allegrone et al developed a method for determining ITX in milk. 50 For the extraction procedure, two alternative methods were assayed. In the first method, the milk was mixed with ethanol and water and extracted with SPE; in the second option, an alkaline hydrolysis was carried out previous to the SPE.…”

Section: Gas Chromatography (Gc)mentioning

confidence: 99%

Analytical Methods for Determining Photoinitiators in Food-Contact Materials

Lago

Sendón

Quirós

2014

Photocured Materials

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In the last decade, European food safety authorities have detected photoinitiators in foodstuffs and packaging. This has led to consumer concerns about the possible risk that these compounds pose to human health. In this context, scientific research groups have developed many different methods for the determination of photoinitiators in food packaging and foodstuffs. This chapter aims to provide a comprehensive overview of all such methods and to recommend the best option for determining photoinitiator molecules. It also includes a comprehensive summary of the state-of-the-art systems for the determination of nonintentionally added substances (NIAS) derived from the photoinitiators. In addition, the present challenges and suggest approaches for dealing with this important problem are discussed.

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“…Extrelut ® 20, Extrelut ® 3 and Extrelut ® 1 columns were purchased from Merck (Darmstadt, Germany). 1,4-Dioxane, (±)-2-phenyl-1-propanol, 2,2′-dithiodibenzoic acid, acetic anhydride, anhydrous aluminium chloride, benzoyl peroxide, bromine, copper(I) bromide, N-bromosuccinimide (NBS), m-chloroperbenzoic acid (mCPBA) (purity: 70%), (diacetoxyiodo)benzene, dichloroethane (DCE), N,N-dimethylformamide (DMF), glacial acetic acid, reduced glutathione (GSH), 2-ITX (as a mixture of 2-and 4-isomers; cLogP: 5.33 ± 0.27 calculated using Advanced Chemistry Development Software version 9.04) (Allegrone et al, 2008), phosphorus tribromide, potassium t-butylate, sulfuryl chloride, thionyl chloride, and triphenylphosphine were used without further purification and were purchased from Sigma-Aldrich. When needed, the reactions were performed in oven-dried glassware under a positive pressure of dry N 2 .…”

Section: Reagents and Chemicalsmentioning

confidence: 99%

In vitrometabolism study of 2-isopropyl-9H-thioxanthen-9-one (2-ITX) in rat and human: evidence for the formation of an epoxide metabolite

2010

Self Cite

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1. 2-Isopropyl-9H-thioxanthen-9-one (2-ITX) is one of the most extensively used photoinitiators in inks found in paper and/or packaging materials for foodstuffs. Recently, traces of 2-ITX as a contaminant were discovered in baby milk and other foodstuffs at a level sufficient to pose a risk to human health. However, little is known about the toxicological profile of 2-ITX. 2. The high lipophilicity of this substance would suggest that it could be a good substrate for hepatic metabolizing enzymes and that these metabolites could have a role in the toxicological properties of 2-ITX. 3. The metabolism of 2-ITX, using both rat and human subcellular preparations, was studied and has resulted in the formation of eight polar metabolites (M1-M8) as revealed in the liquid chromatograpy/ultraviolet (LC/UV) and liquid chromatograpy/mass spectrometry (LC/MS) analyses. Their structures highlight a marked regioselectivity in the metabolism of 2-ITX; it is directed mainly toward the isopropyl moiety and the sulfur atom. 4. The unsaturated metabolite 6 causes the formation of a reactive epoxide metabolite 7. This finding was supported by identification in microsomal incubations of 1,2-diol metabolite 8 arising from the epoxide by hydrolysis and it was validated by incubating in the same conditions the synthetic epoxide 7: the formation of metabolite 8 was again observed. 5. On the basis of these data, we propose that the metabolite 6 could be included in toxicological studies of 2-ITX.

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Development and validation of a solid-phase extraction and gas chromatography–tandem mass spectrometry method for the determination of isopropyl-9H-thioxanthen-9-one in carton packaged milk

Cited by 29 publications

References 7 publications

Evaluation of the migration of 15 photo-initiators from cardboard packaging into Tenax^®using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

Evaluation of the migration of 15 photo-initiators from cardboard packaging into Tenax^®using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

Analytical Methods for Determining Photoinitiators in Food-Contact Materials

In vitrometabolism study of 2-isopropyl-9H-thioxanthen-9-one (2-ITX) in rat and human: evidence for the formation of an epoxide metabolite

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Development and validation of a solid-phase extraction and gas chromatography–tandem mass spectrometry method for the determination of isopropyl-9H-thioxanthen-9-one in carton packaged milk

Cited by 29 publications

References 7 publications

Evaluation of the migration of 15 photo-initiators from cardboard packaging into Tenax®using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

Evaluation of the migration of 15 photo-initiators from cardboard packaging into Tenax®using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

Analytical Methods for Determining Photoinitiators in Food-Contact Materials

In vitrometabolism study of 2-isopropyl-9H-thioxanthen-9-one (2-ITX) in rat and human: evidence for the formation of an epoxide metabolite

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Evaluation of the migration of 15 photo-initiators from cardboard packaging into Tenax^®using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

Evaluation of the migration of 15 photo-initiators from cardboard packaging into Tenax^®using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)