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Mono-methylphthalate MMP (degradation product in urine) Name classification Abbreviation Structureīutyl benzyl BBP phthalate reprotoxic (EPA standard)ĭibutyl phthalate reprotoxic DBP (EPA standard)ĭi-n-octyl phthalate DNOP potential risk (EPA standard)ĭi-isodecyl phthalate DIDP potential riskĭi-(2-ethylhexyl) phthalate DEHP reprotoxic Gradient at 0 minutes 5% B and 5% C, at 2.5 minutes 45% B and 45% Cĭetection: 228/6nm, Reference 380/80nm, 20 Hz, 10-mm cell
#Reference spectrum agilent chemstation plus#
Gradient at 0 minutes 5% B and 5% C, at 10 minutes 45% B and 45% C, at 12.45 minutes 45% B and 45% C, at 12.5 minutes 90% B, at 14 minutes 5% B and 5% Cĭetection 228/6nm, Reference 380/80nm, 20 Hz, 10-mm cellĬhromatographic Conditions for Fast UHPLCĬolumn 1 Agilent ZORBAX RRHT Eclipse Plus Phenyl Hexyl, 2.1° x 50mm, 1.8μm, p/n 959757-912 Gradient 3 at 0 minutes 5% B, 5% C, at 10 minutes 45% B, 45% Cĭetection 228/6 nm, Reference 380/80 nm, 20 Hz, 10-mm cellĬhromatographic Conditions for High-Resolution UHPLCĬolumn 1 Agilent ZORBAX RRHT Eclipse Plus Phenyl Hexyl, 3° x 100mm, 1.8μm, p/n959964-312
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Gradient 2 at 0 minutes 10% C, at 10 minutes 90% C Gradient 1 at 0 minutes 10% B, at 10 minutes 90% B Mobile phases Water (A), Acetonitrile (B), Methanol (C) When the polymers had settled, the solution was filtered through 0.45-μm Agilent Captiva Premium Syringe Filters (regenerated cellulose, p/n 5190-5111), evaporated, and then diluted with 500μL acetonitrile.Ĭhromatographic Conditions for Method DevelopmentĬolumn 1 Agilent ZORBAX Eclipse Plus Phenyl Hexyl, 3° x 100mm, 3.5μm, p/n 959961-312Ĭolumn 2 Agilent ZORBAX Eclipse Plus C-18, 3° x 100mm, 3.5μm, p/n 959961-302 Polymers were precipitated with 10mL of methanol and cooled for 1 hour. In addition, the developed method was transferred to a fast UHPLC method.Īgilent 1290 Infinity Method Development SolutionĬolumn 1 equipped with high pressure G1316C column switching valveĬolumn 2 equipped with low pressure G1316C column switching valveĪ 0.05g amount of the crushed polymer sample was dissolved in 5mL of THF. The performance of the method was evaluated and a real-life sample was measured. In addition, binary and ternary gradients using acetonitrile and methanol as organic phases were applied. A phenyl-hexyl column and a C18 column were used for optimum separation. In the following, a HPLC/UV method was developed for nine phthalates, see Table 1. The German ‘Umwelt Bundesamt’ proposed to replace all phthalate-containing materials, such as flexible PVC, little by little with phthalate-free materials, such as polyethylene and polypropylene, where it is possible. For this reason, their entry into the environment should be prohibited. DINP and DIDP seem to quickly spread in the environment and to enrich in organisms. DEHP, DBP, and BBP were classified as toxic to reproduction and the EU banned them especially from baby products.Ī replacement could be DIDP and DINP for example, which are until now not regarded as toxic, however, these softeners are also forbidden in baby products. Even more strict regulations are under consideration. The 2005/84/EC1 directive lists six phthalates (Table 1) that need to be monitored when used as plasticisers in toys and childcare articles and must be ≤ 0.1% of the mass of the product. Worldwide regulations have been set for allowable levels of phthalates in plastic toys, municipal and wastewater, textiles, and foods.
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In addition, a fast UHPLC method was developed and compared to the high resolution method. Plastic material from a toy was analysed, and the content of phthalates was determined. For the final method precision of retention times and areas, limits of detection (LOD) and limits of quantitation (LOQ), as well as the linearity, was evaluated. An Agilent 1290 Infinity Method Development Solution, in combination with an Agilent Method Scouting Wizard, was used for method development. This Application Note shows the development of an HPLC/UV method for nine phthalates using a phenyl-hexyl column and a ternary gradient. Many official methods are based on GC or GC/MS methods, but during the last decade LC and LC/MS methods were developed. From that time, official authorities in Europe, the US, China, and other countries have passed regulations for phthalates, especially in plastic toys. Since the late nineteen eighties, phthalates have been under suspicion as a health risk for humans.