Department of Environmental Sciences, Faculty of Environmental Studies, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia.
Department of Environmental Sciences, Faculty of Environmental Studies, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia; Laboratory of Halal Science Research, Halal Product Research Institute, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia.
Talanta. 2017 Oct 1;173:51-59. doi: 10.1016/j.talanta.2017.05.064. Epub 2017 May 24.
Estuary sediments are one of the important components of coastal ecosystems and have been regarded as a sink for various types of organic pollutants. Organic pollutants such as endocrine disrupting compounds (EDCs) which have been associated with various environmental and human health effects were detected in the estuary sediment at trace level. Considering various interferences that may exist in the estuarine sediment, a sensitive and selective method, capable of detecting multiclass EDC pollutants at the trace levels, needs to be developed and optimized to be applied for environmental analysis. A combination of Soxhlet extraction followed by offline solid phase extraction (SPE) cleaned up with detection based on LC triple quadrupole MS was optimized and validated in this study. The targeted compounds consisted of ten multiclass EDCs, namely, diclofenac, primidone, bisphenol A, estrone (E1), 17β-estradiol (E2), 17α-ethynylestradiol (EE2), 4-octylphenol (4-OP), 4-nonylphenol (4-NP), progesterone, and testosterone. The method showed high extraction efficiency with percentage of recovery from 78% to 108% and excellent sensitivity with detection limit between 0.02ngg and 0.81ngg. Excellent linearity from 0.991 to 0.999 was achieved for the developed compounds and the relative standard deviation was less than 18%, an indication of good precision analysis. Evaluation of the matrix effects showed ionization suppression for all the developed compounds. Verification of the method was carried out by analyzing the estuarine sediment collected from Langat River. The analyzed estuarine sediments showed a trace concentration of diclofenac, bisphenol A, progesterone, testosterone, primidone, and E1. However, E2, EE2, 4-OP, and 4-NP were below the method's detection limit. Diclofenac exhibited the highest concentration at 2.67ngg followed by bisphenol A (1.78ngg) while E1 showed the lowest concentration at 0.07ngg.
河口沉积物是沿海生态系统的重要组成部分之一，一直被认为是各种类型有机污染物的汇。在河口沉积物中检测到痕量水平的内分泌干扰化合物（EDCs）等有机污染物，这些污染物与各种环境和人类健康影响有关。考虑到河口沉积物中可能存在的各种干扰，需要开发和优化一种灵敏、选择性的方法，以检测痕量水平的多类 EDC 污染物，并将其应用于环境分析。本研究优化并验证了索氏提取结合离线固相萃取（SPE）净化，基于 LC 三重四极杆 MS 检测的方法。目标化合物包括十类多类 EDC，分别为双氯芬酸、扑米酮、双酚 A、雌酮（E1）、17β-雌二醇（E2）、17α-乙炔基雌二醇（EE2）、4-辛基酚（4-OP）、4-壬基酚（4-NP）、孕酮和睾酮。该方法具有较高的提取效率，回收率为 78%至 108%，检测限为 0.02ngg 至 0.81ngg，灵敏度极高。所开发化合物的线性度均在 0.991 至 0.999 之间，相对标准偏差小于 18%，表明分析精度良好。基质效应评价表明，所有开发化合物均存在离子抑制。通过分析从拉让河采集的河口沉积物对方法进行了验证。分析的河口沉积物中痕量存在双氯芬酸、双酚 A、孕酮、睾酮、扑米酮和 E1。然而，E2、EE2、4-OP 和 4-NP 低于方法的检测限。双氯芬酸的浓度最高，为 2.67ngg，其次是双酚 A（1.78ngg），而 E1 的浓度最低，为 0.07ngg。
