ALN-01

1328  B rown et al . : J ournal of AOAC I nternational V ol . 97, N o . 5, 2014

both 0.09 µg/mL, and the LOQs were 0.23 and 0.21 µg/mL, respectively (Table 2).

References

 (1) Haller, J.S. (1990) Bull. N.Y. Acad. Med . 66 , 647–659  (2) Farnsworth, N.R. (1995) NAPRALERT Database , University of Illinois at Chicago, IL, an on-line database available directly through the University of Illinois at Chicago or through the Scientific and Technical Network (STN) of Chemical Abstracts Services  (3) Hecht, A. (1981) FDA Consumer Updates (Issue July-Aug) 15 , 26–29  (4) Tyler, V.E., Bradley, L.R., & Robbers, J.E. (1998) in Pharmacognosy , 9th Ed., Lea & Febiger, Philadelphia, PA, pp 62–63  (5) Bradley, P.R. (1992) in British Herbal Compendium, Vol. 1, British Herbal Medicine Association, Bournemouth, UK, pp 199–203  (6) Reynolds, J.E.F. (1993) in Martindale, the Extra Pharmacopoeia , 30th Ed., Pharmaceutical Press, London, UK, p. 903  (7) Blumenthal, M. (1998) in The Complete German Commission E Monographs: Therapeutic Guide to Herbal Medicines , 12 , 80–81  (8) Beuers, U., Spengler, U., & Pape, G.R. (1991) Lancet , 337–472  (9) Bottenberg, M.M., Wall, G.C., Harvey, R.L., & Habib, S. (2007) Ann. Pharmacother . 41 , 1740–1743. http://dx.doi.org/10.1345/ aph.1K132 (10) NTP Draft Technical Report TR577 (2011) on the Toxicology and Carcinogenesis Studies of a Non-Decolorized Whole leaf extract of Aloe barbadensis Miller ( Aloe vera in F344/N Rats and B6C3F 1 Mice–Drinking Water Study). https://niehs.nih. gov/news/assets/docs_f_o/ntp_draft_technical_report_577_a_ nondecolorized_whole_leaf_extract_of_aloe_barbadensis_ miller_aloe_vera_508.pdf (accessed January 11, 2013) (11) International Aloe Science Council (February 2011) IASC Reference Version 1.0 FAQ. http://www.iasc.org/faq.html (accessed January 11, 2013) (12) Dell’Agli, M., Giavarini, F., Ferraboschi, P., Galli, G., & Bosisio, E. (2007) J. Agric. Food Chem. 55 , 3363–3367. http://dx.doi. org/10.1021/jf070182h (13) El Sohly, M., Gul, W., Avula, B., & Khan, I.A. (2007) J. AOAC Int. 90 , 28–42 (14) Fanali, S., Aturki, Z., D’Orazio, G., Rocco, A., Ferranti, A., Mercolini, L., & Raggi, M.A. (2010) J. Sep. Sci. 33 , 2663–2670. http://dx.doi.org/10.1002/jssc.201000408 (15) Zahn, M., Trinh, T., Jeong, M.L., Wang, D., Abeysinghe, P., Jia, Q., & Ma, W.A (2008) Phytochem. Anal. 19 , 122–126. http:// dx.doi.org/10.1002/pca.1024 (16) Zonta, F., Bogoni, P., Masotti, P., & Micali, G. (1995) J. Chromatogr. A 718 , 99–106. http://dx.doi.org/10.1016/0021- 9673(95)00637-0 (17) Upton, R., Axentiev, P., & Swisher, D. (Eds) (2013) American Herbal Pharmacopoeia and Therapeutic Compendium , AHP, Scott’s Valley, CA, pp 30–33 (18)  Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals (2003) AOAC INTERNATIONAL, Gaithersburg MD (19) Wernimont, G.T. (1987) in Use of Statistics to Develop and Evaluate Analytical Methods , W. Spendley (Ed.), AOAC INTERNATIONAL, Gaithersburg, MD

Precision

From the nine test materials used in this study, five test materials (TM2, TM3, TM5, TM6, and TM8) were above the LOQ and had a HorRat range of 0.3 to 2.0 and RSDr values of 0.61–8.64% as summarized in Table 3. Three of the test materials (TM1, TM7, and TM9) were below the LOQ but were detected, and the one test material (TM4) was below the LOD; therefore, no HorRat and RSD r values were reported for these materials.

Accuracy

The average recovery range of aloin A and aloin B in both solid and liquid matrixes was 84.41–108.86% with an RSD r of 0.15–8.64%. Tables 4a and b contain the summarized results for each individual aloin at the three different concentration levels.

Stability of Mixed Standard

The stability of the aloins in reference standards, as well as test material solutions, was found to be higher with the addition of an acid. It was determined during method optimization that 0.1% acetic acid was adequate to provide good peak shape and retain analyte stability over a period of time. Storage of the aloin reference standards with the addition of an acid provided consistent peak area after 48 h when exposed to room temperature conditions with an average difference of 2–3% mAu*s. In the nonacidified solutions, the aloins started to degrade after 8 h at room temperature, and with an average difference of 23–28% mAu*s after 48 h from the initial time point. This method for the determination of aloin A and aloin B in raw materials and select finished products containing A. vera leaf juice was subjected to an SLV study according to AOAC INTERNATIONAL guidelines. All parameters investigated in the validation study were in compliance with the AOAC INTERNATIONAL guidelines. The described method is thus considered to be suitable for its purpose and ready for further validation studies. Conclusions

Acknowledgments

We would like to acknowledge Aloecorp (Ontario, CA), International Aloe Science Council (Silver Spring, MD) and Mark Roman from Tampa BayAnalytical Research (Tampa Bay, FL) for providing the materials for this study. In addition, we would like to acknowledge the ChromaDex for supplying the reference standards used in the validation study.

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