nutraceutical
Applications
note
Restek Corporation • (800)356-1688 • (814)353-1300 •
#59136
nutraceutical
The Institute for Nutraceutical Advancement (INA)ValidatesGCMethods for
SawPalmettoUsingRtx
®
-5 andStabilwax
®
Columns
History of the INAMethodsValidationProgram
Consumer demand for natural products anddietary supplements
has grown exponentially,with increasing amounts of botanical
materials beingused in themanufacture of a large varietyof
products.As the supplies andnumber of suppliersmultiply, the
consistencyof rawmaterials has become an issue for virtually
everymajor player in thenatural products industry. Even
companieswith conscientious and responsiblequality control
procedures have found it difficult to ensure consistency in their
products due to the lackof anypublished standards for analysis.
These issues, alongwithother science andmarket-based factors,
led29 companies to come together in an international effort to
validate andmake available analyticalmethods thatwillmeet the
demand for global consistency in the testingof botanicals.
The effort is called theMethodsValidationProgram, orMVP,
and it is the first project for the newly formed Institute for
NutraceuticalAdvancement
(INA). INA is anon-corporate
divisionofDenver-based Industrial Laboratories, an independent
laboratory that provides analytical and consulting services to the
natural products industry.
The INAMVP is beingdevelopedunder the directionof a broad
rangeof representatives fromwithin thenatural products
industry, including suppliers,manufacturers, retailers,marketing
companies, agrower and an independent laboratory. Companies
fromboth theUnitedStates andEurope are represented. In
addition, tenmajor natural products organizations, including the
Food andDrugAdministration (FDA), have accepted seats on
the INAMVPAdvisoryCommittee as awayof ensuring that the
process is inclusive. (Additional information is available at
.)
All currentlyvalidatedmethods from the INA canbe viewed at
theirwebsite:
.
Althoughmanyusehighperformance liquidchromatography
(HPLC), twomethods involvegas chromatography (GC) for the
analysis of fatty acids and sterols in sawpalmetto. This fruit
contains several principles thought tohavephysiological activity,
including fatty acids such as caproic, capric, lauric,myristic,
oleic, palmitic, stearic, and1 to2% essential oils. Furthermore,
sawpalmetto contains phytosterols andhighmolecularweight
polysaccharides such as ß-sitosterol, ß-sitosterol 3-O-ß-D-
glucoside, campesterol, stigmasterol. Purified ethanolicorCO
2
extracts of sawpalmettousually contain70 to80% free fatty
acids.The fatty acids present are in several forms: free fatty
acids, fatty acid esters of the fatty alcohols, and fatty acid esters
of thephytosterols.This oil is commonlyblendedwith excipi-
ents to form a drypowder at 30% free fatty acids concentration.
Determination of FattyAcids inSerenoaRepens
(SawPalmetto or Sabel) byGC
This assay canbe used todetermine fatty aciddistribution in saw
palmetto fruit, oil extract, andblendedpowders.Determination is
performedusingGC, after transesterificationof the triglycerides
into themethyl esters occurs. Formore specific informationon
themethod itself and all procedures involved, please refer to
The fatty acids from sawpalmetto are separated inFigure 1,
whichwas obtainedusing aRestekStabilwax
®
column and a
ShimadzuGC-14AGC,with split injection and a flame ioniza-
tiondetector (FID). TheStabilwax
®
columnoffers thenecessary
efficiency and selectivity toprovide accurate identificationof the
fatty acids (asmethyl esters).
Figure1
The Stabilwax
®
columnoffers the necessary efficiency and
selectivity toprovide accurate identificationof the fatty
acids (asmethyl esters).
50m, 0.25mm ID, 0.25µm Stabilwax
®
(cat.# 10626-105). 1µL split
injection.
Oven temp.:
110°C (hold 1min.) to 240°C@ 8°C/min.
(hold 25min.);
Inj./FID temp.:
230°C/250°C;
Carrier gas:
Hydrogen
@ 2.5mL/min.;
Split flow:
37.5mL/min.;
Septum purge:
3mL/min.
20
min.
10
30
87
10
6
9
11
12
1 2 3 4 5
1. caproic acid
2. caprylic acid
3. pelargonic acid
4. capric acid
5. lauric acid
6. myristic acid
7. palmitic acid
8. margaric acid
9. stearic acid
10. oleic acid
11. linoleic acid
12. linolenic acid
