A simple and convenient HPLC-FD detection method for ochratoxin A (OTA) with a high detection limit and a short run time has been developed. OTA has been found in most samples of Chinese market wine, including domestic and imported wines, but the content was not very high. Only a few wines showed an OTA content that exceeded the EC and OIV limits, indicating that most Chinese market wines were safe. The OTA intake for Chinese from wine was 0.017 ng/kg (bw) per day, which was lower than the SCF and JECFA limits and also lower than in many other countries. This was mainly due to the low per capita wine consumption in China, but it is still necessary for the Chinese government and wine makers to monitor OTA levels in wine and to establish relevant regulations. An egg white treatment (0.20 mg/mL, 48 h) was the best removal method for OTA.
Jingyuan Shao,Wen Cao,Haibin Qu,Jianyang Pan,Xingchu Gong
The aim of this study was to present a novel analytical quality by design (AQbD) approach for developing an HPLC method to analyze herbal extracts. In this approach, critical method attributes (CMAs) and critical method parameters (CMPs) of the analytical method were determined using the same data collected from screening experiments. The HPLC-ELSD method for separation and quantification of sugars in Codonopsis Radix extract (CRE) samples and Astragali Radix extract (ARE) samples was developed as an example method with a novel AQbD approach. Potential CMAs and potential CMPs were found with Analytical Target Profile. After the screening experiments, the retention time of the D-glucose peak of CRE samples, the signal-to-noise ratio of the D-glucose peak of CRE samples, and retention time of the sucrose peak in ARE samples were considered CMAs. The initial and final composition of the mobile phase, flow rate, and column temperature were found to be CMPs using a standard partial regression coefficient method. The probability-based design space was calculated using a Monte-Carlo simulation method and verified by experiments. The optimized method was validated to be accurate and precise, and then it was applied in the analysis of CRE and ARE samples. The present AQbD approach is efficient and suitable for analysis objects with complex compositions.
危险品化学品经营许可证（带存储）