Ooshima Tomoko, Kakutani Naoya, Yamaguchi Yukihiko, Kawakami Tsuyoshi
Osaka Institute of Public Health.
National Institute of Health Sciences.
Yakugaku Zasshi. 2022;142(3):279-287. doi: 10.1248/yakushi.21-00197.
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 and TDBPP-d, 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.
根据《含有有害物质的家庭用品控制法》，日本禁止在窗帘、地毯和睡衣等纺织产品中使用阻燃剂，即双（2,3-二溴丙基）磷酸酯（BDBPP）和三（2,3-二溴丙基）磷酸酯（TDBPP）。在此，我们开发了一种基于气相色谱-质谱联用（GC-MS）的方法，以比现行官方方法更高的准确性和安全性来定量这些化合物。为了进行准确和灵敏的定量，使用氘代化合物BDBPP-d和TDBPP-d作为替代标准品。考虑到分析人员的安全，对预处理中使用的某些致癌或有爆炸风险的溶剂和试剂进行了更换。对于萃取步骤，用乙酸乙酯替代了苯，对于甲基衍生化步骤，试剂从自行制备的重氮甲烷乙醚溶液改为己烷中的三甲基硅基重氮甲烷溶液，这是一种安全且易于使用的市售试剂。甲基化的BDBPP（BDBPP-Me）和TDBPP的校准曲线在0.5 - 8.0 μg/mL范围内呈线性。BDBPP-Me的检测限为0.05 μg/g，TDBPP的检测限为0.3 μg/g，与目前BDBPP-Me的10 μg/g和TDBPP的8 μg/g的检测限相比足够低。当向0.5 g样品中添加5 μg BDBPP和TDBPP时，各种窗帘材料中的回收率为66 - 108%，相对标准偏差为1.2 - 10.2%。因此，所开发的方法适用于各种材料的纺织产品。
