Chromatography Forum

Need detection analysis of multiple raw herbs (alflafa, astragalus, cayenne, celery, parsley, pau d'arco). FDA will want quant. Have HP1100 DAD, gradient method can easily separate many peaks, but nothing unique for each for quantification. Too small for UV detection we believe. Could ELSD (expensive) or CAD work? And, any other suggestions? Thank you!

Need detection analysis of multiple raw herbs (alflafa, astragalus, cayenne, celery, parsley, pau d'arco). FDA will want quant.

Why would FDA care about stuff which are non-pharmaceutical ingredients? I've done FDA/cGMP work for 30 years and never have come across anything like this.

100% identity testing is now required according to FDA's Dietary Supplement GMPs. Since FDA believes there are no "active" ingredients, each and every ingredient must be tested. The industry knows this is bogus but FDA requires it. FDA does have procedures for possible exemption*, however part of the petition is to demonstrate through testing that testing is not necessary. First, the testing has to be presented. There are no identity tests that would differentiate these herbs (that I know of) so we were looking at HPLC analysis. We are analyzing by HPLC anyway for another ingredient in the product that we consider the active ingredient.
*Petition to Request an Exemption From 100 Percent Identity Testing of Dietary Ingredients: Current Good Manufacturing
Practice in Manufacturing, Packaging, Labeling or Holding Operations for Dietary Supplements, 72 Fed. Reg. 34,959
(June 25, 2006) (to be codified at 21 C.F.R. pt. 111).

Even in green salade are more pharmaceutical active compounds than we all would believe. Please google on the websites of HPLC column manufacturers and look for brochures called "Nutraceuticals" or "Food and Beverages" analysis. Or contact the company Phytochem in Germany, Neu-Ulm. http://www.phytochem-standards.de/! They are experts in herbs analysis, and familiar with FDA requierments. The person there is Hans Rausch. Give him my regards and good luck.
Their full address is:
Phytochem®
Referenzsubstanzen GbRmbH
Hans Rausch, Biologist and Chemist
Dipl. Biol. Dr. Klaus Denzel, Dr. Andreas Hofmann
Krumbacher Straße 9
D - 89335 Ichenhausen
Germany

Phone: 0049 -731/972 05-45
Fax: 0049 -731/972 05-46
e-mail: phytochem@t-online.de

Development laboratory:
Reuttier Straße 56
D - 89231 Neu-Ulm
Germany

Identity test of complex dry samples... That sounds like a perfect task for near-infrared spectroscopy (if you happen to have one of those in your lab).

It sounds hopeless do this with LC/UV and compare retention times of unknown compounds - in a chromatogram filled with thousands of peaks. LC/MS is probably a better option if you want to stick with LC.

NIR is a good idea -- we do not have one, but will look into that method! Otherwise we were thinking of analyzing for a specific marker compounds for each herb. Thanks to all -- I appreciate it!

100% identity test require that you have a set of "authentic" standards to compare with. As long as you use the same methodology for both standards and samples, either LC-DAD or IR (the most popular two) or other techniques such as TIC and LC-MS will work. The difficult part is that you need set the acceptance criteria.

It is not to require you to identify each unknown peak.

Very true! We have decided to perform the identity test by gradient HPLC-DAD on the sample and compare peaks with the standard prepared from the combination herbal mixture. The sample (and each raw material) should easily match the standard peaks and satisfy FDA identity requirements. We will be fine as long as they do not want us to assay each herb. NIR looked good but it is an expense and the method would still need developed. HPLC is easy and we are already running it for other ingredients in the sample. Thanks yangz00g and to all!