[Analysis of Flame Retardants Bis(2,3-dibromopropyl) phosphate and Tris(2,3-dibromopropyl) phosphate in Textile Products by GC-MS].

The use of flame retardants, namely bis(2,3-dibromopropyl) phosphate (BDBPP) and tris(2,3-dibromopropyl) phosphate (TDBPP), in textile products such as curtains, carpets and sleeping clothes is banned in Japan under the 'Act on the Control of Household Products Containing Harmful Substances'. Herein, we developed a GC-MS based method to quantify these compounds with greater accuracy and safety than the current official method. For accurate and sensitive quantification, deuterated compounds, BDBPP-d ₁₀ and TDBPP-d ₁₅ , were used as surrogate standards. In consideration of the safety of the analyst, certain solvents and reagents used for the pretreatment that are carcinogenic or have a risk of explosion were replaced. For the extraction step, benzene was replaced by ethyl acetate, and for the methyl derivatization step, the reagent was changed from a self-prepared solution of diazomethane in ether to a solution of trimethylsilyl diazomethane in hexane, a safe and easy-to-use commercially available reagent. The calibration curves were liner in the range of 0.5-8.0 μg/mL for both methylated BDBPP (BDBPP-Me) and TDBPP. The detection limit was 0.05 μg/g for BDBPP-Me and 0.3 μg/g for TDBPP, which is sufficiently low compared to the current detection limits of 10 μg/g for BDBPP-Me and 8 μg/g for TDBPP. The recoveries in various curtain material were 66-108% and relative standard deviations were 1.2-10.2% when 5 μg BDBPP and TDBPP were added to 0.5 g of samples. Thus, the developed method is applicable to textile products of various materials.