Determination of MCPD and glycidyl esters in foodstuff with the CHRONECT Workstation MCPD and the module ISO 18363-1
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Determination of MCPD and glycidyl esters in foodstuff with the CHRONECT Workstation MCPD and the module ISO 18363-1

CHRONECT Workstation MCPD – Module ISO 18363-1 Application note 1603 Introduction 3-Monochloro-1,2-propanediol (3-MCPD), 2monochloro-1,3-propanediol (2-MCPD) and glycidol belong to the group of manufacturing-related contaminants in food. MCPD fatty acid esters can be formed during refining at high temperatures in the presence of chloride-containing salts. However, refining is a necessary chemical and physical refining process in the production of many oils. It is only through this temperature treatment that undesirable odors and flavors, as well as any traces of toxic compounds such as...

CHRONECT Workstation MCPD – Module ISO 18363-1 Application note 1603 Device setup for the "DGF Fast & Clean" method The instrument setup for the "DGF Fast & Clean" method is shown schematically in Figure 2. For the automation of the sample preparation Axel Semrau chooses a 160 cm CHRONECT Robotic DHR, because it offers enough space for all necessary modules and can easily be adapted to all other methods and further applications. However, a variant with a 120 cm CHRONECT Robotic RTC is also possible. The dilutor is equipped with two solvents (n-hexane and extraction agent). For this...

CHRONECT Workstation MCPD – Module ISO 18363-1 Application note 1603 For example, the 3-in-1 method (AOCS Cd 29b13 or ISO 18363-2) can be automated. In this case, an additional cooling tray for -22 °C is incorporated. For the Unilever method (AOCS Cd 29a-13 or ISO 18363-3), a centrifuge and an evaporation unit can be added and integrated. This method, like the Zwagerman method (Draft ISO 18363-4), can thus be easily automated. The older Weisshaar method has also been implemented. Figure 3: Section of the CHRONOS software platform: Overlapping mode of operation and sample result after 48...

CHRONECT Workstation MCPD – Module ISO 18363-1 Application note 1603 Table 1: Measuring parameters of the triple quadrupole for the detection of 3-MCPD and 2-MCPD. SSL, 1 µL injektion volume, splitless (split 1:30 after 1 min) Heating rate [°C/min] Pressure regulation Analytical column Oven program 1.5 mL/min constant flow, backflush on after 8.5 min 2x Rxi-5 MS 15 m, 0.25 mm inner diameter, 0.25 µm film Heating rate [°C/min] Transfer line 280 °C, CID gas argon, MRM mode Table 2: Recovery (RC in %) and reproducibility (RP in %) of the methods "DGF classic" and "DGF Fast & Clean" for part A...

CHRONECT Workstation MCPD – Module ISO 18363-1 Application note 1603 Table 3: Results of the validation of a CHRONECT Workstation MCPD in a routine laboratory with a set LOQ of 0.05 mg/kg fat. Validation parameter System precision Calibration 0.05 – 0.5 mg/kg 0.5 – 5.0 mg/kg LOQ 0.05 mg/kg Linearity 0.05 / 2.0 / 10 mg/kg Accuracy Reproducibility Validation data Criterion for characteristics of the method Part A Part B Part A Part B Part A Part B Part A Part B Table 4: Contents of a reference oil from FAPAS (T2646QC) according to the "DGF classic" and "DGF Fast & Clean" methods as well as...

CHRONECT Workstation MCPD – Module ISO 18363-1 Application note 1603 based on measurements on four consecutive days. The validation of the method "DGF Fast & Clean" according to the EU commission (Table 3) additionally shows the achievement of all necessary criteria for the use of this method in routine e.g. for the release analysis of a production refinery. Looking at the range of values from the interlaboratory comparison for the reference oil FAPAS 2646 (3-MCPD 0.352 - 0.821 mg/kg), it can be seen that there seem to be significant deviations between laboratories of +/- 40 % in the...

CHRONECT Workstation MCPD – Module ISO 18363-1 Application note 1603 Example measurements Figure 6 and Table 5 show an excellent comparability of the methods "DGF classic", "DGF Fast & Clean" and the 3-in-1 method. Compared to manual sample preparation, "DGF Fast & Clean" in particular leads to considerable time savings. In the meantime, more than 100 different matrices have been successfully measured with the "DGF Fast & Clean" in routine applications. This includes normal oils and fats as well as extracts of compound food as shown in Figure 6. In order to make the method even more...

CHRONECT Workstation MCPD – Module ISO 18363-1 Application note 1603 Summary 2- and 3-MCPD as well as glycidol are present as contaminants in our food. Due to their high carcinogenicity, their analysis is becoming more and more important. The rapidly growing demand requires an automation of analytical methods in order to increase throughput and reproducibility. The implementation shown here in the form of the "DGF Fast & Clean" method enables a statement to be made in a short time, approx. 48 minutes for a sample with Part A and Part B. Axel Semrau therefore recommends "DGF Fast & Clean" as...