Organophosphorus flame retardants are a class of widely used plasticizers and flame retardants. In this study, an analytical methodology for the simultaneous determination of 13 organophosphorus flame retardants in milk was developed by using high-performance liquid chromatography-tandem mass spectrometry in combination with a modified quick, easy, cheap, effective, rugged, and safe technique and solid-phase extraction. The experimental parameters of the sample purification procedure and high-performance liquid chromatography-tandem mass spectrometry were optimized. The developed method was validated in terms of linearity, limits of detection, recovery, and precision. The method showed a linear response in the 1–100 ng/mL concentration range and the limits of detection ranged from 0.001 to 0.3 ng/mL. The mean recoveries for most organophosphorus flame retardants were in the ranges of 75.0–115.8% (spiked at 2.5 ng/mL) and 76.7–124.8% (spiked at 25 ng/mL), with relative standard deviations of <13.09%. The developed methodology was successfully applied to the analysis of nine human milk samples and nine commercial cow milk samples. Eleven organophosphorus flame retardants were detected in the human milk samples, with median concentrations that ranged from lower than the limit of detection to 1.47 ng/mL, and only nine organophosphorus flame retardants were detected in cow milk samples, with median levels of <0.32 ng/mL.

中文翻译：

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使用改进的快速、简便、廉价、有效、耐用且安全的技术、固相萃取和 HPLC-MS/MS 快速测定牛奶中的 13 种有机磷阻燃剂

有机磷阻燃剂是一类应用广泛的增塑剂和阻燃剂。在本研究中，通过使用高效液相色谱-串联质谱法结合改进的快速、简便、廉价、有效、耐用且安全的技术，开发了一种同时测定牛奶中 13 种有机磷阻燃剂的分析方法，固相萃取。优化了样品纯化程序和高效液相色谱-串联质谱的实验参数。开发的方法在线性、检测限、回收率和精密度方面得到验证。该方法在 1–100 ng/mL 浓度范围内显示出线性响应，检测限范围为 0.001 到 0.3 ng/mL。大多数有机磷阻燃剂的平均回收率在 75.0–115.8%（加标为 2.5 ng/mL）和 76.7–124.8%（加标为 25 ng/mL）的范围内，相对标准偏差 <13.09%。所开发的方法已成功应用于 9 种人乳样品和 9 种商业牛奶样品的分析。在人乳样品中检测到 11 种有机磷阻燃剂，中值浓度范围从低于检测限到 1.47 ng/mL，而牛奶样品中仅检测到 9 种有机磷阻燃剂，中值水平<0.32 ng /毫升。所开发的方法已成功应用于 9 种人乳样品和 9 种商业牛奶样品的分析。在人乳样品中检测到 11 种有机磷阻燃剂，中值浓度范围从低于检测限到 1.47 ng/mL，而牛奶样品中仅检测到 9 种有机磷阻燃剂，中值水平<0.32 ng /毫升。所开发的方法已成功应用于 9 种人乳样品和 9 种商业牛奶样品的分析。在人乳样品中检测到 11 种有机磷阻燃剂，中值浓度范围从低于检测限到 1.47 ng/mL，而牛奶样品中仅检测到 9 种有机磷阻燃剂，中值水平<0.32 ng /毫升。