SPDS Lutein and Turmeric ERPs

For linearity ‐ yes. For analytical range ‐ mostly, but limited to 25%, but does not meet the range  requirements of greater than 50% (there are products out there that high). For LOQ ‐  the SMPR specifies that the LOQ should be less than 0.1% in the sample  materials. The LOQ specified in this method is ug/mL. using the lowest dilution for  this method the curcumin (which is the highest LOQ ‐ 2.86 ug/mL) would back  calculate to 0.0143 %, assuming that the sample mass is 500 mg, which is not  actually specified in the method (taken from optimization information). So Yes, LOQ  is sufficient. Accuracy/Recovery ‐ Not specified in the document. Repeatability ‐ As specified above the methodology used biases the repeatability  data due to between injection and between sample being treated as replicates.  Additionally, the CurcuViva product is consistently not within the <5% RSDr as  specified in the SMPR. All other products appear to meet SMPR repeatability  requirements, but I would recommend re‐treating the data and only taking the  triplicate measurements to ensure true repeatability is obtained. Some of the other dietary ingredients listed in Table 2 have also not been used in  any of the multi‐component products.

3.  Is there information  demonstrating that the method  performs within the SMPR Method  Preformance Requiements table  specifications for all analytes in the  SMPR applicability statement?  If  not, please specify what is missing  and whether or not the method's  applicaiblity should be modified.  

1.  Based on the supporting  information, were there any  additional steps in the evaluation  of the method that indicated the  need for any addional  precautionary statements in the  method? 2.  Does the method contain  system suitability tests or controls  as specified by the SMPR?  If not,  please indicate if there is a need  for such tests or controls, and  which ones. 3.  Is there information  demonstrating that the method  system suitability tests and  controls as specified in the SMPR  worked appropriately and as  expected?  If no, please specify. 4.  Based on the supporting  information, is the method written  clearly and concisely?  If no, please  specify the needed revisions. IV.  General Submission Package

No

The system suitability requirements of the SMPR specifies that check standards  should be run throughout the validation ‐ in the case of this run, there were only  blank samples, but no QC/check standards run. System suitability was not performed  at the beginning of the validation either to ensure that the system was working  properly. Linearity was sufficient, which would ensure that the system was suitable, but there  was no actual system suitability performed.

There is some information that is missing in the method preparation. The actual  sample masses of the samples (or atleast recommended ranges of masses) are  missing. This would cause a lot of confusion adopting the method. Additionally,  several different extraction volumes were used. It would make sense to specify  which volumes were suitable for what types of samples (or what expected ranges or  ingredients). As for softgels, the results obtained from this would likely be  mg/capsule, rather than mg/g, as you should not typically include the mass of the  softgel in the analysis.

5.  Based on the supporting  information, what are the  pros/strenghts of the method?

The strengths: simple sample preparation fast chromatographic separation baseline separation of the curcuminoids suitable for many sample types, ingredients, etc. The weaknesses: lack of sufficient information for sample preparation

6.  Based on the supporting  information, what are the cons  /weaknesses of the method?

requires a significant amount of glassware extraction solvent selection (see below)