Lee Isaac, Gao Quanyin, Liu Wei, Patel Darshan, Smith Malissa, You Hong, Patel Tushar, Aylozyan Karine, Babajanian Silva, Collins Teddy, Sullivan Darryl, Chang Peter, Swanson Gary
Herbalife Manufacturing LLC, Quality Control, 20481 Crescent Bay Drive, Lake Forest, CA, 92630, United States.
Herbalife Nutrition, Quality Control, 950 West 190th St, Torrance, CA, 90502, United States.
J AOAC Int. 2025 May 1;108(3):449-471. doi: 10.1093/jaoacint/qsae070.
A multilaboratory validation study was performed on AOAC Official Method 2016.09, for final action. Eight different laboratories throughout the world participated in the study and tested the same set of six different laboratory samples of raw materials (commercial) and formulated products (commercial), and all the laboratories successfully generated results within the acceptance criteria.
The intention of the study was to evaluate specificity, precision (variation), linearity/range, system suitability, LOD, and LOQ by multiple laboratories to satisfy the requirement for moving Official Method 2016.09 to final action status. Accuracy and ruggedness were already validated in earlier work through single-laboratory validation, and it was not necessary to include these validation parameters in the multilaboratory validation study.
Laboratory samples containing Aloe vera were sent out to participating laboratories. Each laboratory followed Official Method 2016.09 (First Action) to analyze the content of aloin A, aloin B, and aloe-emodin using HPLC. The results generated by each laboratory were collected and evaluated.
The specificity results show that blank and matrix chromatograms do not contain major interfering peaks at the retention time of aloin A, aloin B, and aloe-emodin. The precision (variation) results of duplicated preparations are not more than 0.05 parts per million (ppm) different. The linearity/range results from six standards (10 parts per billion [ppb], 20 ppb, 40 ppb, 80 ppb, 160 ppb, and 500 ppb) have correlation coefficient (R) values of ≥0.999. The system suitability results meet the acceptance criteria to show the instrument validity. The LOD results show that the S/N ratios of the 10 ppb standards for all three components are about 3. The LOQ results show that the S/N ratios of 20 ppb standards for all three components are about 10.
The parameters (specificity, precision [variation], linearity/range, system suitability, LOD, and LOQ) have been validated and show that the test method is suitable for its intended use.
The test method has been successfully validated by eight different laboratories around the world (United States, United Kingdom, Germany, and Canada). Each of the laboratories is managed independently by a site laboratory management team. This multilaboratory study has validated Official Method 2016.09 (First Action) and the method is fit for its intended purpose.
针对AOAC官方方法2016.09进行了一项多实验室验证研究，以确定最终方法。全球八个不同实验室参与了该研究，测试了同一组六种不同的原材料（商业样品）和配方产品（商业样品）实验室样品，所有实验室均成功得出符合验收标准的结果。
该研究旨在通过多个实验室评估特异性、精密度（变异性）、线性/范围、系统适用性、检测限（LOD）和定量限（LOQ），以满足将官方方法2016.09推进至最终方法状态的要求。准确性和耐用性在早期工作中已通过单实验室验证，因此无需在多实验室验证研究中纳入这些验证参数。
将含有库拉索芦荟的实验室样品分发给参与研究的实验室。每个实验室按照官方方法2016.09（初法），使用高效液相色谱法（HPLC）分析芦荟苷A、芦荟苷B和芦荟大黄素的含量。收集并评估每个实验室得出的结果。
特异性结果表明，空白和基质色谱图在芦荟苷A、芦荟苷B和芦荟大黄素的保留时间处不包含主要干扰峰。重复制剂的精密度（变异性）结果差异不超过百万分之0.05（ppm）。六个标准品（十亿分之十[ppb]、20 ppb、40 ppb、80 ppb、160 ppb和500 ppb）的线性/范围结果的相关系数（R）值≥0.999。系统适用性结果符合验收标准，表明仪器有效。检测限结果表明，所有三种成分10 ppb标准品的信噪比约为3。定量限结果表明，所有三种成分20 ppb标准品的信噪比约为10。
各参数（特异性、精密度[变异性]、线性/范围、系统适用性、检测限和定量限）均已得到验证，表明该测试方法适用于其预期用途。
该测试方法已由全球八个不同实验室（美国、英国、德国和加拿大）成功验证。每个实验室均由当地实验室管理团队独立管理。这项多实验室研究验证了官方方法2016.09（初法），该方法适用于其预期目的。
