Advances in GC-MS/MS Enhance Routine Detection of Dioxins and Dioxin-like Compounds in Food and Animal Feed


Dioxins are extremely poisonous natural compounds that may stay within the surroundings for prolonged intervals. These persistent natural pollution (POPs), which embrace polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs), are primarily generated by the combustion or manufacture of chlorine-containing supplies resembling plastics. Dioxins and different carefully associated POPs, resembling polychlorinated biphenyls (PCBs), are classed as carcinogenic by the US Environmental Safety Company, and current a big menace to human well being even at low ranges.

Dioxins and PCBs can enter the meals chain when livestock eat contaminated animal feed, and might accumulate within the fatty tissues of animals as a consequence of their excessive fat-solubility. Consequently, over 90% of human publicity to dioxins and PCBs is thru the consumption of meat, fish, dairy and different meals of animal origin.1 Given the well being dangers posed by dioxins and PCBs, efficient meals testing workflows are important to make sure merchandise don’t exceed regulatory-defined secure ranges.

GC-MS/MS: A Strong Method for Analyzing Dioxins and PCBs in Meals and Animal Feed

To manage human publicity to PCDDs, PCDFs and PCBs from the meals chain, international regulatory our bodies have established most ranges (MLs) and motion ranges (ALs) for numerous POPs in meals merchandise, in addition to permitted analytical strategies for meals testing laboratories to implement these requirements. Within the European Union (EU), for instance, European Fee laws 2017/644 and 2017/771 define sampling, pattern preparation and evaluation protocols for the detection of dioxins and different dioxin-like compounds in meals and animal feedstuffs.2,three

With meals testing laboratories tasked with dealing with probably a whole lot of samples daily, these workflows have to be supported by strong and dependable analytical applied sciences that may confidently determine and precisely quantify dioxins and PCBs with minimal upkeep necessities with the intention to decrease downtime and maximize throughput.

Due to ongoing enhancements within the robustness and sensitivity of fuel chromatography-triple quadrupole mass spectrometry (GC-MS/MS) methods, laws had been up to date in 2014 to allow this system as a substitute for fuel chromatography-high decision mass spectrometry (GC-HRMS) for confirmatory evaluation and for the management of MLs and ALs. The most recent GC-MS/MS methods are able to exceptionally dependable efficiency for the routine evaluation of dioxins and PCBs, offering correct and delicate quantification of those compounds even at hint ranges.

Case Research: Delicate and Dependable Dedication of Dioxins Utilizing GC-MS/MS

The efficiency of recent GC-MS/MS methods was evaluated in a current examine involving the confirmatory evaluation and quantification of 17 PCDDs and PCDFs, and 18 dioxin-like and non-dioxin-like PCBs in solvent requirements and numerous meals and feedstuff samples. The samples had been analyzed utilizing a triple quadrupole GC-MS/MS system outfitted with the superior electron ionization supply (AEI) and a TG-Dioxin capillary GC column. Two similar GC-MS/MS methods in two separate laboratories had been used to evaluate the reproducibility of the strategy.

Extraction was carried out by Twisselmann scorching extraction or pressurized liquid extraction. The automated clean-up of the extracts was carried out utilizing a three-column setup, comprising multi-layered acidic silica, alumina and carbon columns. Two fractions had been generated per pattern (the primary containing non-ortho PCBs, PCDDs and PCDFs, and the second containing mono-ortho and di-ortho PCBs and indicator PCBs) and these had been analyzed individually. The analytical technique gave wonderful separation of all of the PCDD, PCDF and PCB congeners in lower than 45 minutes.

Given the excessive sensitivity of recent GC-MS/MS devices, a calibration-based strategy was used to find out limits of quantitation (LOQs) of the analytical system. Utilizing calibration requirements on the LOQ and subsequent test requirements at this degree enabled the efficiency of the strategy to be assessed all through the analytical sequence. This additionally allowed LOQs for the person congeners to be decided, assuming a set pattern weight. Particular person congener LOQs may very well be utilized to upper-bound, middle-bound and lower-bound toxicity equivalence (TEQ) outcomes by substituting the results of any congener that fell beneath the bottom calibration level with this worth multiplied by the toxicity equivalence issue (TEF) of the congener.

To guage the response issue deviation over the course of the analytical sequences, requirements on the specified LOQ had been analyzed at the beginning, throughout and finish of every run. Utilizing a nominal weight of two g, and assuming 100% 13C-labeled customary restoration and all natives had been lower than the LOQ within the pattern, a minimal upper-bound worth of zero.152 pg/g WHO-PCDD/F-TEQ was decided. This met regulatory necessities for reporting at 1/fifth of the ML upper-bound sum TEQ for all meals and feedstuffs with a nominal consumption of two g, excluding steerage related to liver of terrestrial animals and meals for infants or younger youngsters, which each have authorized limits outlined on a contemporary weight foundation. In these circumstances, both a bigger pattern consumption or a magnetic sector instrument could be required. The entire calibration sequences demonstrated response issue %RSDs inside EU laws, highlighting the suitability of the strategy.

To reveal the efficiency of the GC-MS/MS system, six replicate extractions of a combined fats high quality management pattern (QK1) had been ready, break up between the 2 websites and analyzed at common intervals all through the analytical sequences (14 injections in whole). The measured WHO-PCDD/F-TEQ values for congener had been in wonderful settlement with the reference worth offered by the EU Reference Laboratory for Halogenated POPs in Feed and Meals, and the higher certain WHO-PCDD/F-TEQ worth didn’t deviate by greater than 6% from the reference worth for all 14 measurements (Determine 1). The deviation between the upper-bound and lower-bound WHO-PCDD/F-TEQ for every measurement was persistently lower than 1.2%, effectively beneath the utmost restrict of 20% essential to help compliance with EU laws.

pper- and lower-bound WHO-PCDD/F-TEQ valuesDetermine 1. Higher- and lower-bound WHO-PCDD/F-TEQ values for all 14 measurements of the QK1 combined animal fats high quality management pattern, for six replicate extractions.

Strong Routine Evaluation of Dioxin and Dioxin-like Compounds

To evaluate the robustness of the GC-MS/MS system, the PCDD, PCDF and non-ortho PCB extracts had been pooled right into a combined matrix pattern and analyzed greater than 161 injection sequences throughout a interval of roughly two weeks. Every sequence consisted of 40 matrix injections and 40 LOQ requirements, interspersed with nonane blanks. No system upkeep, tuning or person intervention was undertaken all through the two-week examine. Determine 2 highlights the distinctive peak space stability achieved for chosen PCDD and PCDF congeners.

Peak area repeatabilityDetermine 2. Absolute peak space repeatability over two weeks of study for chosen PCDD and PCDF congeners in a pooled matrix pattern (%RSD and quantities on column are proven for every congener).

These outcomes spotlight the distinctive ranges of day-to-day measurement repeatability provided by the newest GC-MS/MS methods. By delivering persistently excessive efficiency with out the necessity for in depth upkeep steps, fashionable GC-MS/MS methods are maximizing instrument uptime and growing pattern throughput for routine POP evaluation workflows.


Developments in GC-MS/MS know-how, particularly the superior electron ionization supply, are pushing the bounds of measurement sensitivity, repeatability and robustness to help the wants of routine dioxin and PCBs evaluation in meals and feed samples. By minimizing instrument downtime whereas sustaining distinctive ranges of analytical efficiency, these superior methods are serving to high-throughput meals testing laboratories to investigate extra samples and in the end higher shield shoppers from these dangerous pollution.


Malisch, R. and Kotz, A. (2014) Dioxins and PCBs in feed and meals – Evaluation from European perspective. Sci Whole Environ, 491, 2-10.
European Fee. Fee Regulation (EU) 2017/644, Off J Eur Union, 2017, L92 9-34.
European Fee. Fee Regulation (EU) 2017/771, Off J Eur Union, 2017, L115 22-42.


This text relies on analysis by Richard Regulation and Cristian Cojocariu (Thermo Fisher Scientific, Runcorn, UK), Alexander Schaechtele (EU Reference Laboratory for Halogenated POPs in Feed and Meals, Freiburg, Germany), Amit Gujar (Thermo Fisher Scientific, Austin, US), and Jiangtao Xing (Thermo Fisher Scientific, Beijing, China).

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