In this study, we describe a high-throughput and sensitive method for textiles analysis, using liquid chromatography coupled to quadrupole-Orbitrap high resolution mass spectrometry (LC-Q-Orbitrap HRMS), for the simultaneously quantitative analysis of 40 target alkylphenol polyethoxylates (APEO) oligomers with reference standards and screening of 160 alcohol polyethoxylates (AEO) oligomers without standards in textiles. The APEOs contain nonylphenol ethoxylates (NPEOs) and octylphenol ethoxylates (OPEOs) with an EO number of ethylene oxide of 1–20, while AEOs focus on C₁₁EOs-C₁₈EOs with an EO number of 1–20. After ultrasonic extraction in methanol, the extract was directly separated using a core-shell CORTECS C₁₈⁺ column and analyzed by Full MS/dd-MS² (data dependent acquisition) scan in ESI positive mode. Two best sensitivity experimental conditions for APEOs with short EO chains (AP(EO)_1-2) and long EO chains (AP(EO)_3-20) were investigated, respectively. Most APEO oligomers had wide concentration ranges and the correlation coefficients (R²) were higher than 0.999. The limit of quantitation (LOQ) values for NP(EO)_3-20 oligomers ranges from 16.00 to 52.80 μg/kg and for OP(EO)_3-20 oligomers is from 2.40 to 8.00 μg/kg. LOQ for NP(EO)₁ and NP(EO)₂, OP(EO)₁ and OP(EO)₂ was 2.40 mg/kg and 0.24 mg/kg, 1.20 mg/kg and 0.16 mg/kg, respectively. The average recovery for each APEO oligomer in cotton and polyester matrix was between 78% and 110% at three spiked levels and the relative standard deviation (RSD%) was below 10%. As to AEOs suspects, a HRMS compound database containing 160 AEO oligomers was built and several parameters such as exact m/z, isotopic patterns, predicted product ions and predicted retention time were used for screening and confirmation. The established method was successfully applied for analysis of 40 commercial textile samples. Compared with OPEOs, NPEOs, especially NP(EO)_3-15 oligomers, were widely detected in samples and the total concentration ranged from 1.56 to 1376.31 mg/kg. AEOs were also found in most samples, among which C_12-14, C₁₆ and C₁₈ compounds appeared more frequently and the EO chains mainly ranged from 3 to 15.

在这项研究中，我们描述了一种高通量，灵敏的纺织品分析方法，该方法采用液相色谱与四极杆Orbitrap高分辨率质谱联用（LC-Q-Orbitrap HRMS），用于同时定量分析40种目标烷基酚聚乙氧基化物（APEO） ）具有参考标准的低聚物，并筛选出纺织品中没有标准的160种醇聚乙氧基化物（AEO）低聚物。APEO包含壬基酚乙氧基化物（NPEO）和辛基酚乙氧基化物（OPEO），环氧乙烷的EO数为1至20，而AEO集中于EO数为1至20的C ₁₁ EOs-C ₁₈ EO。在甲醇中超声提取后，使用核壳CORTECS C ₁₈ ⁺直接分离提取物色谱柱，并以ESI阳性模式通过Full MS / dd-MS ²（数据相关采集）扫描进行分析。分别研究了具有短EO链（AP（EO）_1-2）和长EO链（AP（EO）_3-20）的APEO的两个最佳灵敏度实验条件。大多数APEO低聚物的浓度范围很广，相关系数（R ²）高于0.999。NP（EO）_3-20低聚物的定量极限（LOQ）值为16.00至52.80μg/ kg，OP（EO）_3-20低聚物的定量极限为2.40至8.00μg / kg。NP（EO）₁和NP（EO）₂，OP（EO）₁和OP（EO）_2的LOQ分别为2.40 mg / kg和0.24 mg / kg，1.20 mg / kg和0.16 mg / kg。在三个加标水平下，棉和聚酯基质中每种APEO低聚物的平均回收率在78％至110％之间，相对标准偏差（RSD％）低于10％。对于AEO嫌疑人，建立了包含160个AEO低聚物的HRMS化合物数据库，并使用了几个参数（例如精确的m / z，同位素模式，预测的产物离子和预测的保留时间）进行筛选和确认。所建立的方法已成功用于40种商品纺织品样品的分析。与OPEOs相比，NPEOs，尤其是NP（EO）_3-15样品中广泛检测到低聚物，总浓度范围为1.56至1376.31 mg / kg。在大多数样品中还发现了AEO，其中C _12-14，C ₁₆和C ₁₈化合物的出现频率更高，EO链的主要范围为3至15。