30 Ossipee Road
P.O. Box 9101
Newton, MA 02464-9101
Phone: (617) 969-5452
Fax: (617) 965-1213
www.microfluidicscorp.com
Prepared for:
A Nutraceutical Company
Prepared by:
Steven Vincent Mesite
Kenneth John Chomistek
03/09/2011
Company: A nutraceutical company
Product: Curcumin powder for use as a nutraceutical ingredient. Two different types of curcumin were tested, a natural extract and a synthetic type.
Objective: The objective was to produce nanodispersions (0.1-0.4 μm) of curcumin in oil with as high of a solid loading as possible.
Conclusion:
§ The M-110P Microfluidizer® processor was successful in reducing the size of the curcumin powder in several different formulations.
§ The largest particle size reduction was observed with a 5% wt. dispersion of the synthetic curcumin in a 1% wt. Tween 80 in water. The median particle size of this formulation was reduced from 18.46 μm to 0.436 μm after 50 passes through the G10Z (87 μm) interaction chamber (IXC) at 30,000 psi.
§ The synthetic curcumin was also processed in turmeric oil and canola oil at concentrations as high as 50% wt. solids.
Recommendations:
· Process the dispersion with the M-110P, M-110EH, or M-700 Microfluidizer processor.
· Optimize the following processing parameters:
o Formulation (including solid loadings, oil type and surfactant type)
o Processing pressure (20,000 – 30,000 psi)
o Number of passes
· Analyze the processed materials to determine if they meet the desired specifications.
Equipment: Microfluidizer Processor M-110P
Interaction Chambers G10Z (87 μm)
H30Z (200 μm)
Particle Size Analyzer Horiba LA-910
Diluent D.I. water (17.1 megaohms)
Relative Refractive Index 1.06 - 0.10i
Optical Microscope Olympus BH2 with attachments
Rotor Stator Mixer IKA T-25
Procedure: The raw materials were sent to Microfluidics for the testing. A total of seven experiments were performed using the M-110P Microfluidizer processor. The details of the formulation and processing parameters can be found in Table 1.
Table 1. Processing conditions and observations for the customer’s curcumin formulations.
Test# / Formulation / Processing Conditions / Observations20110301A / 5% wt. Tween 20 in turmeric oil
33% wt. natural curcumin / 1 pass H30Z 12,000 psi / Sample plugged the IXC and the inlet check valve
20110301B / 2% wt. Tween 80 in water
5% wt. natural curcumin / 20 passes G10Z 30,000 psi / Sample processed without any issues
20110301C / 1% wt. Tween 80 in water
5% wt. synthetic curcumin / 50 passes G10Z 30,000 psi / Sample processed without any issues
20110301D / 5% wt. Tween 20 in turmeric oil
42% wt. synthetic curcumin / 10 passes G10Z 30,000 psi / Sample became too viscous to process
20110301E / 5% wt. Tween 20 and 5% wt. lecithin in turmeric oil
48% wt. synthetic curcumin / 10 passes G10Z 30,000 psi / Sample became too viscous to process
20110302A / 5% wt. Span 20 and 5% wt. lecithin in turmeric oil
50% wt. synthetic curcumin / 20 passes G10Z 30,000 psi / Sample became too viscous to process
20110302B / 5% wt. Span 20 and 5% wt. lecithin in canola oil
50% wt. synthetic curcumin / 20 passes G10Z 30,000 psi / Sample became too viscous to process even after heating to 44ºC
Analysis: The samples with water as the continuous phase of the dispersion were analyzed using the Horiba LA-910 particle size analyzer. The diluent used for particle size analysis was water. All samples were analyzed using an optical microscope.
Results: A table listing particle size data can be found in Table 2. Representative particle size distributions from the aqueous trials can be found in Figure 1. Representative microscope pictures can be found in Figures 2-8.
Table 2. Particle size distributions from the customer’s Curcumin in water tests. The sample highlighted in green was the smallest sample produced.
d10 / d50 / d90
20110301B / Unprocessed / 0.538 / 30.01 / 345.7
1 / 0.421 / 3.016 / 12.62
5 / 0.346 / 1.020 / 4.746
10 / 0.359 / 0.895 / 2.001
20 / 0.360 / 0.726 / 1.281
20110301C / Unprocessed / 1.920 / 18.46 / 41.31
1 / 0.393 / 1.243 / 7.706
5 / 0.364 / 0.807 / 2.143
10 / 0.341 / 0.615 / 1.306
20 / 0.333 / 0.528 / 1.175
50 / 0.297 / 0.436 / 0.887
Figure 1. Particle size distributions from test 20110301C, the 5% wt. curcumin 1% wt. Tween 80 solution test.
Unprocessed
Figure 2. Microscope pictures from test 20110301A before processing. These particles clogged the inlet check valve of the processor.
Unprocessed 1 pass G10Z 30,000 psi
5 passes G10Z 30,000 psi 20 passes G10Z 30,000 psi
Figure 3. Microscope pictures from test 20110301B before and after various stages of processing.
Unprocessed 1 pass G10Z 30,000 psi
20 passes G10Z 30,000 psi 50 passes G10Z 30,000 psi
Figure 4. Microscope pictures from test 20110301C before and after various stages of processing.
1 pass G10Z 30,000 psi
5 passes G10Z 30,000 psi 10 passes G10Z 30,000 psi
Figure 5. Microscope pictures from test 20110301D after various stages of processing.
1 pass G10Z 30,000 psi
5 passes G10Z 30,000 psi 10 passes G10Z 30,000 psi
Figure 6. Microscope pictures from test 20110301E after various stages of processing.
Unprocessed 5 passes G10Z 30,000 psi
10 passes G10Z 30,000 psi 20 passes G10Z 30,000 psi
Figure 7. Microscope pictures from test 20110302A before and after various stages of processing.
Unprocessed 5 passes G10Z 30,000 psi
10 passes G10Z 30,000 psi 20 passes G10Z 30,000 psi
Figure 8. Microscope pictures from test 20110302B before and after various stages of processing.
Comments:
§ The samples with the synthetic curcumin all processed without any plugging problems.
§ For the oil samples, as the particle size of the curcumin decreased, the viscosity of the dispersions increased. This caused some feeding problems as the viscosity became very high.
§ The formulation (% solids, % and type(s) of surfactant) needs to be optimized to limit this viscosity increase so that the sample can be processed sufficiently to achieve the desired particle size.
§ It may be possible to use PureNano crystallization technology to achieve the target particle size with less energy input.
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