GC-MS Analysis of Tris(1-aziridinyl)phosphine Oxide Flame Retardants in Textile Products

Abstract

Tris(1-aziridinyl)phosphine oxide (APO) used as flame retardant in textile products, such as curtains, carpets, and sleeping clothes, is prohibited in Japan under the "Act on the Control of Household Products Containing Harmful Substances." This study developed a GC-MS-based method to quantify APO more accurately and safely than the current official method. The APO in textile products was extracted with methanol, the extract was replaced with acetone instead of hexane as previously reported, and purified by florisil cartridge column. This cleanup method was instead of the harmful and carcinogenic dichloromethane used for open column to purify the sample in the official method, giving consideration to health of analysts. For accurate and sensitive quantification, deuterated compound, APO-d12, was used as a surrogate standard. The calibration curve displayed linearity within the 0.01-2.0 µg/mL range for APO. The detection limit for APO was 0.008 µg/g with S/N=5, which was 50 times more sensitive than the current detection limit of 0.4 µg/g, enabling the analysis of sufficiently low concentrations. The recoveries in non-treatment cloth and flame-retardant textiles were 73.5-126.6% and relative standard deviations were 3.3-24.6% when 2 µg APO was added to 0.5 g of samples, confirming that it can be analyzed satisfactorily. Thus, the developed method is applicable to textile products of various materials.