Method development on automated sample preparation system for content uniformity and assay testing in a product with multiple APIs and new strategy for quick development and application.

Automation of analytical sample preparation and testing is always attractive due to its high efficiency and continuous operation, but it can also be very challenging due to the operational complexity and method development. Studies focused on method development in automated systems are extremely rare and little has been published on the subject. In this paper, we investigate several unique and advanced aspects of this subject. The example product is selected containing two APIs to be tested by a single method to be productive. The product strengths of the two APIs are significantly different, making development of a single method much more challenging. In addition, we use a "green chemistry" approach, avoiding any organic solvent in the dissolving media in order to achieve an environmentally friendly solution. The selection and optimization of several key operational parameters are then discussed. The successful method is achieved using a new strategy called "Automated Online Standard (AO-STD)" methodology. This novel approach is compared to the manual operation procedure. The proposed approach can substantially reduce the method transfer time, generally considered the biggest obstacle to practical deployment of automated systems. The automated system applied in this paper is most suitable for content uniformity testing, but is also applicable for potency assays, blend uniformity testing, and degradation product tests.

Assay of active pharmaceutical ingredients in drug products based on relative response factors: Instrumentation insights and practical considerations.

Relative Response Factors (RRFs) can be used for quantitation of one compound against another and it is widely used for Impurity analysis of pharmaceutical products; however, the application in potency assay is limited. Through an extensive study shown in this paper, it can be concluded that using the "RRF methodology" for potency assay is much more challenging compared to impurity analysis, due to the much tighter criteria required for potency analysis. The effects of instrument settings, which are rarely discussed or recognized in current HPLC analytical method development and quality release testing, are discussed. These factors impact the RRF just as much as other commonly recognized HPLC parameters. The effects of UV detector settings, i.e. Slit Width, Step Width, Band Width, and Data Collection Module, have been explored. This phenomenon has been demonstrated using three compounds to observe the impact of their quantitation due to the significant RRF variations. Finally, principles to reduce RRF variations have been discussed, and practical considerations of RRF application to method development and method transfer are provided.

Urgent need to improve the quality of case report in traditional Chinese medicine: Assessment on reporting quality of 3,417 cases / 中国结合医学杂志

<p><b>OBJECTIVE</b>To survey the reporting quality of traditional Chinese medicine (TCM) case reports published in recent years and understand the common problems. The assessment results would lay the foundation for the development of recommendations for case report in Chinese medicine.</p><p><b>METHODS</b>This survey determined the reporting quality of cases with Chinese herbal decoction, Chinese proprietary medicine, acupuncture, moxibustion and other traditional therapies published in 20 core medical journals of China by searching the China Academic Journals Full-text Database from 2006 to 2010. Fifty survey items in 16 domains were used to determine the reporting quality. One point was assigned to each item (Yes=1 point; No=0 point), and total score was 50 points. The domain of treatment was assessed independently, ranging from 2 to 9 items for different TCM interventions.</p><p><b>RESULTS</b>The total of 1,858 case reports, covering 3,417 cases were included to analyze from 13 out of 20 core medical journals of China. There were 74.8% of them did not identify the nature of study in title, while 73.9% did not comprise an abstract. Incomplete reporting was found in discussions/ comment, and only 38.9% had made recommendations or take-away messages. Figures and tables were infrequently used. Three cases cited the full names of patients, but without declaring that any consent was obtained. Over 90% reported the symptoms and signs of TCM, and characteristics on tongue and pulse, but less than 50% did mention other medical history and diagnostic rationale. More than 90% treatments of the included cases were herbal decoction, with clear reporting on the ingredients and dosages. However, the reporting rate of the dosages of each ingredient was just 48.4%. Almost none reported the quality control of crude herbs, manufacturers and lot numbers of herbal proprietary medicine. Besides, advices and precautions on diet, emotions and living were rare to be illustrated.</p><p><b>CONCLUSION</b>Systematic reporting recommendations are urged to develop for improving the contents and format of case reports in TCM.</p>

Improving the quality of randomized controlled trials in Chinese herbal medicine, part IV: applying a revised CONSORT checklist to measure reporting quality / 中西医结合学报

OBJECTIVE: To discuss the quality of reporting in randomized controlled trials (RCTs) of Chinese herbal medicine (CHM), and to provide suggestions for improving the reporting of future clinical studies in this therapeutic area. METHODS: A search of the Cochrane Library was conducted to identify RCTs of CHM. A revised CONSORT checklist designed for CHM clinical studies was implemented. The revised CONSORT checklist contained 63 items, including the following new items added specifically for CHM: (1) "syndrome of disease" based on Chinese medicine theories; (2) rationale of CHM formula; (3) formula composition; (4) preparation form of CHM; (5) quality control of CHM. RESULTS: The overall reporting quality of the RCTs as assessed with the revised CONSORT checklist varied between 19% and 44%, with a median score of 32% (standard deviation 8%). CONCLUSION: The overall quality of reporting of RCTs of CHM evaluated with a revised CONSORT checklist was poor, reflecting the need for improvements in reporting future clinical trials in this area. RECOMMENDATIONS: To improve the quality of reporting of RCTs of CHM, we recommend adopting a revised CONSORT checklist that includes items specific to CHM. We also recommend that editors of CHM journals require authors to use a structured approach to presenting their trials as a condition of publication.