Expert Review Panel for Dietary Supplements

IV. General Submission Package 1. Based on the supporting information, were there any additional steps in the evaluation of the method that indicated the need for any additional 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. 5. Based on the supporting information, what are the pros/strengths of the method? 6. Based on the supporting information, what are the cons/weaknesses of the method?

The rreeport's Results and Discussion section stated, "The resolution was >1.5 for 7-OH mitragynine and mitragynine to close eluting components (Figure 2)", however, no 7-OH mitragynine peak is seen in Figure 2 at the scales presented. This is followed with a description of requiring the use of spiked samples to monitor acceptable separation of the target analytes. If accepted, the official method should include this monitoring step and how to respond if the target analytes are not resolved from interference. Also, the protocol on how to evaluate if a separation is acceptable.

The method describes their evaluation of potential interferences but should add requirements on acceptable chromatographic separations.

Comfrey leaves were used as blank check samples. Standards were obtained from 2 sources. For the low and midpoint of analytical range, these ranges were not well described as explained in Section II Part 2. Calibration solution chromatography results, peak areas versus concentrations, were not tabulated or plotted. The correlation coefficients were reported as all being >99.9% but seeing the data is requested. The sample prep needs to be made clearer: "Samples were centrifuged at 4500 rpm for 5 min. The dried extract contained a high concentration of mitragynine, therefore a 1:10 dilution was performed with methanol". If the extract was truly dried, the reconstitution volume is needed. If "dried" is removing the 10 mL extraction liquid from the solid material, then the 1:10 makes sense. This must be clarified.

System suitability of chromatography should be listed.

The method is quite simple and uses standard analytical equipment. It can can be performed quickly.

Analytical range of analytes in original materials need to be stated. Need system suitability for chromatographic separation. LOD/LOQ must be properly determined by spiking blank matrix at low levels. Clarification of 1:10 dilution of dried extract in the sample preparation.

Specific details for these are listed earlier in this report.

7. Any general comments about the method?

No additional comments.

Recommendation for the Method

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