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Development and validation of a multi-residue method for the simultaneous analysis of brominated and organophosphate flame retardants, organochlorine pesticides, and polycyclic aromatic compounds in household dust
Analytical Methods ( IF 2.7 ) Pub Date : 2021-09-15 , DOI: 10.1039/d1ay00860a Wenrui Zhang 1 , Yonghui Wang 1 , Meilu Hao 1 , Biao Kong 1 , Peng Liang 2 , Yan Yang 3 , Shengtao Ma 3
Analytical Methods ( IF 2.7 ) Pub Date : 2021-09-15 , DOI: 10.1039/d1ay00860a Wenrui Zhang 1 , Yonghui Wang 1 , Meilu Hao 1 , Biao Kong 1 , Peng Liang 2 , Yan Yang 3 , Shengtao Ma 3
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Household dust is a sink for multiple toxic chemicals with known or suspected potential health effects. However, most dust exposure studies focus on a few chemicals, which may limit overall understanding of human exposure characteristics because people spend most of their time indoors. This paper describes the development and evaluation of a multi-residue analysis of 20 organochlorine pesticides (OCPs), 15 polycyclic aromatic hydrocarbons (PAHs), 8 polybrominated diphenyl ether congeners (PBDEs), 3 hexabromocyclododecane (HBCDs), 8 synthetic musks (Musks), and 7 organophosphate esters (OPEs) in indoor dusts. After extraction with acetone/hexane (v/v, 1 : 1), all target compounds were fractionated with a Florisil solid-phase extraction (SPE) cartridge into two fractions: PAHs, PBDEs, HBCDs, OCPs and Musks, which were eluted with hexane/dichloromethane, and OPEs eluted with ethyl acetate. Further clean-up using acidified silica 44% cartridges was then performed to enable determination of PBDEs and HBCDs. Instrumental analysis of the target chemicals was performed using gas chromatography (GC) or liquid chromatography (LC) coupled with mass spectrometry (MS) or tandem mass spectrometry (MS/MS). A newly-optimized GC-MS/MS method was employed for the simultaneous determination of PAHs, OCPs, and Musks. The lower limit of quantification (LOQ) values of PAHs, OCPs, and Musks were 0.14–0.92 ng g−1, 0.06–0.38 ng g−1 and 0.07–0.40 ng g−1, respectively. PBDEs were quantified by GC-MS with electron capture negative ionization, and HBCDs and OPEs by LC-MS/MS with electrospray ionization (ESI) in negative and positive ion mode, respectively. Recovery experiments showed that the average recoveries and relative standard deviations were 99–113% and 1–14% for PBDEs, 89–105% and 1–6% for HBCDs, 71–120% and 3–17% for PAHs, 71–112% and 2–17% for OCPs, 77–120% and 2–13% for Musks, and 80–127% and 1–14% for OPEs. Validation experiments showed that the method achieved good accuracy. The developed method was used to analyze SRM 2585 and real indoor dust samples to demonstrate its suitability for routine analysis. The target contaminants were widely detected in SRM 2585 and indoor dust collected from Wuhan of Central China, with PAHs the major species, followed by OPEs, OCPs, and PBDEs.
中文翻译：
用于同时分析家庭灰尘中溴化和有机磷阻燃剂、有机氯农药和多环芳族化合物的多残留方法的开发和验证
家庭灰尘是多种已知或怀疑具有潜在健康影响的有毒化学物质的汇。然而，大多数粉尘暴露研究都集中在少数化学品上，这可能会限制对人类暴露特征的整体理解，因为人们大部分时间都在室内度过。本文介绍了对 20 种有机氯农药 (OCP)、15 种多环芳烃 (PAH)、8 种多溴二苯醚同系物 (PBDE)、3 种六溴环十二烷 (HBCD)、8 种合成麝香 (Musks) 进行多残留分析的开发和评估和 7 种室内灰尘中的有机磷酸酯 (OPE)。用丙酮/己烷 (v/v, 1 : 1) 萃取后，所有目标化合物用 Florisil 固相萃取 (SPE) 柱分离成两个部分：PAHs、PBDEs、HBCDs、OCPs 和 Musks，用己烷/二氯甲烷洗脱，OPE用乙酸乙酯洗脱。然后使用酸化二氧化硅 44% 小柱进行进一步净化，以测定多溴二苯醚和六溴环十二烷。使用气相色谱 (GC) 或液相色谱 (LC) 结合质谱 (MS) 或串联质谱 (MS/MS) 对目标化学品进行仪器分析。采用新优化的 GC-MS/MS 方法同时测定 PAH、OCP 和麝香。PAH、OCP 和麝香的定量下限 (LOQ) 值为 0.14–0.92 ng g 使用气相色谱 (GC) 或液相色谱 (LC) 结合质谱 (MS) 或串联质谱 (MS/MS) 对目标化学品进行仪器分析。采用新优化的 GC-MS/MS 方法同时测定 PAH、OCP 和麝香。PAH、OCP 和麝香的定量下限 (LOQ) 值为 0.14–0.92 ng g 使用气相色谱 (GC) 或液相色谱 (LC) 结合质谱 (MS) 或串联质谱 (MS/MS) 对目标化学品进行仪器分析。采用新优化的 GC-MS/MS 方法同时测定 PAH、OCP 和麝香。PAH、OCP 和麝香的定量下限 (LOQ) 值为 0.14–0.92 ng g-1 , 0.06–0.38 ng g -1和 0.07–0.40 ng g -1， 分别。PBDEs 通过 GC-MS 与电子捕获负离子化，HBCDs 和 OPEs 通过 LC-MS/MS 与电喷雾电离 (ESI) 分别在负离子和正离子模式下进行定量。回收率实验表明，PBDEs 的平均回收率和相对标准偏差分别为 99-113% 和 1-14%，HBCDs 为 89-105% 和 1-6%，PAHs 为 71-120% 和 3-17%，71- OCP 为 112% 和 2-17%，麝香为 77-120% 和 2-13%，OPE 为 80-127% 和 1-14%。验证实验表明，该方法取得了良好的准确性。开发的方法用于分析 SRM 2585 和真实的室内灰尘样品，以证明其适用于常规分析。目标污染物在华中地区武汉采集的 SRM 2585 和室内灰尘中广泛检测到，其中 PAHs 是主要种类，其次是 OPEs、OCPs 和 PBDEs。
更新日期：2021-09-20
中文翻译：
用于同时分析家庭灰尘中溴化和有机磷阻燃剂、有机氯农药和多环芳族化合物的多残留方法的开发和验证
家庭灰尘是多种已知或怀疑具有潜在健康影响的有毒化学物质的汇。然而，大多数粉尘暴露研究都集中在少数化学品上，这可能会限制对人类暴露特征的整体理解，因为人们大部分时间都在室内度过。本文介绍了对 20 种有机氯农药 (OCP)、15 种多环芳烃 (PAH)、8 种多溴二苯醚同系物 (PBDE)、3 种六溴环十二烷 (HBCD)、8 种合成麝香 (Musks) 进行多残留分析的开发和评估和 7 种室内灰尘中的有机磷酸酯 (OPE)。用丙酮/己烷 (v/v, 1 : 1) 萃取后，所有目标化合物用 Florisil 固相萃取 (SPE) 柱分离成两个部分：PAHs、PBDEs、HBCDs、OCPs 和 Musks，用己烷/二氯甲烷洗脱，OPE用乙酸乙酯洗脱。然后使用酸化二氧化硅 44% 小柱进行进一步净化，以测定多溴二苯醚和六溴环十二烷。使用气相色谱 (GC) 或液相色谱 (LC) 结合质谱 (MS) 或串联质谱 (MS/MS) 对目标化学品进行仪器分析。采用新优化的 GC-MS/MS 方法同时测定 PAH、OCP 和麝香。PAH、OCP 和麝香的定量下限 (LOQ) 值为 0.14–0.92 ng g 使用气相色谱 (GC) 或液相色谱 (LC) 结合质谱 (MS) 或串联质谱 (MS/MS) 对目标化学品进行仪器分析。采用新优化的 GC-MS/MS 方法同时测定 PAH、OCP 和麝香。PAH、OCP 和麝香的定量下限 (LOQ) 值为 0.14–0.92 ng g 使用气相色谱 (GC) 或液相色谱 (LC) 结合质谱 (MS) 或串联质谱 (MS/MS) 对目标化学品进行仪器分析。采用新优化的 GC-MS/MS 方法同时测定 PAH、OCP 和麝香。PAH、OCP 和麝香的定量下限 (LOQ) 值为 0.14–0.92 ng g-1 , 0.06–0.38 ng g -1和 0.07–0.40 ng g -1， 分别。PBDEs 通过 GC-MS 与电子捕获负离子化，HBCDs 和 OPEs 通过 LC-MS/MS 与电喷雾电离 (ESI) 分别在负离子和正离子模式下进行定量。回收率实验表明，PBDEs 的平均回收率和相对标准偏差分别为 99-113% 和 1-14%，HBCDs 为 89-105% 和 1-6%，PAHs 为 71-120% 和 3-17%，71- OCP 为 112% 和 2-17%，麝香为 77-120% 和 2-13%，OPE 为 80-127% 和 1-14%。验证实验表明，该方法取得了良好的准确性。开发的方法用于分析 SRM 2585 和真实的室内灰尘样品，以证明其适用于常规分析。目标污染物在华中地区武汉采集的 SRM 2585 和室内灰尘中广泛检测到，其中 PAHs 是主要种类，其次是 OPEs、OCPs 和 PBDEs。
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