DCA quality analysis

DCA packages

We have tested dichloroacetate packages of four different suppliers for toxic substances and other impurities. Our analysis shows that the purest Sodium Dichloroacetate is from DCA-LAB. The packages with the most impurities are from PureDCA and PharmaDCA. Sodium Dichloroacetate from PharmaDCA has high amount of toxic substances.

OBJECT OF RESEARCH

Dichloroacetate packages of four different suppliers were used for the research:

Brand Company Product Lot/Batch number Expiration date
DCA-LAB Curaltus Ltd 25 gr. DCA Powder Lot No: D16-C1-2/25 March, 2018
Sigma-Aldrich Sigma-Aldrich Chemie GmbH 10 gr. DCA Powder LOT# STBD9074V -
Pharma DCA A.W.P. Ltd 20 gr. DCA Powder Batch No 01780 November, 2017
Pure DCA / theDCAstore - 20 gr. DCA Powder LOT: 72641 September, 2016

ANIONIC CHROMATOGRAPHY

Anionic dichloroacetate composition was measured using Ionic chromatograph with DCA solution.

590 mg of DCA powder was used for the research, all of which was dissolved in 1 lliter of distilated water (H2O conductivity - 5 mkS). Thus solutions were obtained, each of which contained 590 mg / l sodium dichloroacetate, equivalent to 500 mg of dichloroacetate anion in 1 liter of water.

Prepared solutions (590 mg/l) were examined using an ionic chromatograph through anionic column. The column and detector standardly calibrated for fluoride, chloride, nitrite, bromide, nitrate, phosphate, sulfate anions. Also additionally calibrated for dichloroacetate (Cl2CH-COO-), monochloroacetate (ClCH2-COO-), glyoxylate (OCH-COO-) for anions and identification peaks were determined of other potential impurities: glycolate (HOCH2-COO-), oxalate (-OOC-COO-) anions.

The results are presented in the table ranked from best to worst:

Rank Brand Dichloroacetae
concentracion, mg/l
Dichloroacetate
anion, mg/l
Monochloroacetate
anion, mg/l
Glyoxylate
anion, mg/l
Glycolate anion Oxalate anion Chloride anion
1 DCA-LAB 590 500.93 0.09 - - Traces Traces
2 Sigma-Aldrich 590 501.09 0.35 - - Traces Traces
3 Pure DCA 590 446.85 0.36 0.21 Visible peak Visible peak Visible peak
4 Pharma DCA 590 484.26 1.40 - - Visible peak Visible peak

Note: The chloride anion gives a peak of 0,45 µS in an empty water sample so we did not assess it quantitatively; it is certain that Sigma Aldrich and DCA-LAB products have an insignificant amount of chloride anion.

Anion chromatography charts of every product:
DCA-LAB
Sigma-Aldrich
Pure DCA
Pharma DCA

HEADSPACE GAS CHROMATOGRAPHY (HS-GC)

Volatile halogenated hydrocarbons (Determination of highly volatile halogenated hydrocarbon) were measured using HS-GC chromatograph with DCA solution.

590 mg of DCA powder was used for the research, all of which was dissolved in 1 lliter of distilated water (H2O conductivity - 5 mkS). 5 ml of the obtained solutions were diluted  to 500 ml (100 times), resulting in solution that contains 5,9 mg/l of sodium dichloroacetate, which is equivalent to 5 mg dichloroacetate anions in 1 liter of water.

Prepared DCA solutions (5,9 mg/l) were examined using HS-GC method, heating the solution at  90 oC temperature. This method allows you to precisely examine the amount of dissolved halogenated hydrocarbons in an aqueous solution: chloroform, bromdichlormetan, chlordibrommetan, bromoform, trichloreten, tetrachloreten, at a concentration between 0.1 μg/l and 2 μg /l.

The results are presented in the table ranked from best to worst:

Rank Brand Dichloroacetae
concentracion, mg/l
Chloroform, µg/l Bromodichloromethane, µg/l Chlorodibromomethane, µg/l Bromoform, µg/l Trichloroethene, µg/l Tetrachloroethene, µg/l
  Pure water 0 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10
1 DCA-LAB 5,9 0.10 <0.10 <0.10 <0.10 <0.10 <0.10
2 Pure DCA 5,9 0.13 <0.10 <0.10 <0.10 <0.10 <0.10
3 Sigma-Aldrich 5,9 0.46 <0.10 <0.10 <0.10 <0.10 <0.10
4 Pharma DCA 5,9 0.63 <0.10 <0.10 <0.10 <0.10 <0.10

HS-GC charts of every product:
Pure water
DCA-LAB
Sigma-Aldrich
Pure DCA
Pharma DCA

SUMMARY

Summarized results of the Anionic chromatography and HS-GC (Headspace Gas chromatography) are presented in the table ranked from best to worst. Table columns show dichloroacetate amount (%) and amounts of measured impurities: toxic monochloroacetate (ppM), toxic chloroform (ppM) and other impurities (glycolate, glyoxilate, oxalate, chloride) and H2O amount (%). Visual evidence of mechanical impurities is also assessed.

Rank Brand DCA amount
advertised, %
DCA amount
determined, %
Monochlororacetate
anion amount, ppM
Chloroform
amount, ppM
Other impurities
+ H2O, %
Mechanical
impurities
1 DCA-LAB 99 99,98 153 17 0,00 Traces
2 Sigma-Aldrich 98 99,93 593 78 0,00 Traces
3 Pure DCA 99 89,35 610 22 10.58 Strongly noticealbe
4 Pharma DCA 99 96,83 2373 107 2.92 Strongly noticealbe

CONCLUSIONS

  1. Sodium Dichloroacetate packages from DCA-LAB and Sigma-Aldrich matches parameters advertised by the supplier.
  2. Sodium Dichloroacetate packages from PureDCA and PharmaDCA doesn't match advertised parameters.
  3. The purest Sodium Dichloroacetate is from DCA-LAB.
  4. Sodium Dichloroacetate with the most impurities is from PureDCA and PharmaDCA.
  5. Sodium Dichoroacetate from PharmaDCA has high amount of toxic substances.