A high-throughput analytical method for complex contaminant mixtures in biosolids

Abstract

Biosolids are rich in organic matter and other nutrients that contribute to environmental and agricultural sustainability by improving soil textural and biological properties and enhancing plant growth when applied to agricultural crops. Land application of biosolids encourages resource recovery and circumvents drawbacks associated with landfilling or incineration. However, biosolids contain numerous chemicals at trace levels, and quantitative analysis of such mixtures in this complex matrix is crucial for understanding and managing application risks. There are currently few analytical methods available that are capable of extracting and quantifying a large range of the emerging contaminants found in biosolids. In this study, a simplified, rapid, and robust method of analysis was developed and validated for a high-priority organic contaminant mixture of 44 endocrine disrupting compounds known to occur in biosolids. Analytes consisted of chemicals from many classes with a wide range of physiochemical properties (e.g., log K_ow values from -1.4 to 8.9). The biosolids extraction and cleanup protocol was validated for 42 of the targeted compounds. The UPLC-MS² parameters were validated for all 44 organic contaminants targeted for study. From the two batches of biosolids tested using this analytical method, most of the targeted contaminants (86%) were detected with 100% frequency at concentrations ranging from 0.036 to 10,226 μg/kg dw. Performance results highlighted that internal standards alone could not negate biosolids matrix effects; thus, internal standards and the standard addition method were used for residue quantification. This was the first study to detect and quantify 6PPD-q in biosolids, and the first to quantify lidocaine and 11 other chemicals in biosolids using a single analytical method. This method may be expanded for analysis of additional chemicals in biosolids and comparable matrices.

Keywords: Biosolids extraction methods; Chemical mixtures; Complex matrices; Endocrine disrupting compounds analysis; Multi-class; Multi-residue analysis; UPLC-MS(2) analysis.