Discoursing on Soxhlet extraction of ginseng using association analysis and scanning electron microscopy

Soxhlet extraction is a common method of sample preparation. However, there has been no discussion about the efficiency of Soxhlet extraction from different batches and the factors that cause content fluctuation. In this study, Panax ginseng was selected as a model sample. Soxhlet extraction by means of a water bath, which has always been neglected, was identified as a novel key factor in the poor repeat- ability in different batches of Soxhlet extraction, as it can affect the siphon times and reflux time, which have been positively correlated with the ginsenoside contents. By substituting round bottom flasks in the same column, the relative standard deviation of the most fluctuated compound, ginsenoside Rbl, was decreased from 24.6% to 5.02%. Scanning electron microscopy analysis confirmed that the breakdown of the surface of the ginseng powder in the Soxhlet extraction led to a better dissolution of ginsenosides, indicating that chloroform may promote the extraction of ginsenosides by disrupting the cell structure. Moreover, 70% methanol was regarded as the better solvent for extracting the ginsenosides. Overall, this work offers a practical and effective protocol for improving the accuracy and repeatability of Soxhlet extraction methodology for ginsenosides and other analytes.

Real-time toxicity prediction of Aconitum stewing system using extractive electrospray ionization mass spectrometry

Due to numerous obstacles such as complex matrices,real-time monitoring of complex reaction systems(e.g.,medicinal herb stewing system)has always been a challenge though great values for safe and rational use of drugs.Herein,facilitated by the potential ability on the tolerance of complex matrices of extractive electrospray ionization mass spectrometry,a device was established to realize continuous sampling and real-time quantitative analysis of herb stewing system for the first time.A complete analytical strategy,including data acquisition,data mining,and data evaluation was proposed and implemented with overcoming the usual difficulties in real-time mass spectrometry quantification.The complex Fuzi(the lateral root of Aconitum)-meat stewing systems were real-timely monitored in150 min by qualitative and quantitative analysis of the nine key alkaloids accurately.The results showed that the strategy worked perfectly and the toxicity of the systems were evaluated and predicated accordingly.Stewing with trotters effectively accelerated the detoxification of Fuzi soup and reduced the overall toxicity to 68%,which was recommended to be used practically for treating rheumatic arthritis and enhancing immunity.The established strategy was versatile,simple,and accurate,which would have a wide application prospect in real-time analysis and evaluation of various complex reaction systems.

Limitation standard of toxic aconitines in Aconitum proprietary Chinese medicines using on-line extraction electrospray ionization mass spectrometry

Development of rapid analytical methods and establishment of toxic component limitation standards are of great importance in quality control of traditional Chinese medicine. Herein, an online extraction electrospray ionization mass spectrometry(oEESI-MS) coupled with a novel whole process integral quantification strategy was developed and applied to direct determination of nine key aconitine-type alkaloids in 20 Aconitum proprietary Chinese medicines(APCMs). Multi-type dosage forms(e.g., tablets, capsules, pills, granules, and liquid preparation) of APCM could be determined directly with excellent versatility. The strategy has the characteristics of high throughput, good tolerance of matrix interference, small amount of sample(~0.5 mg) and reagent(~240 μL) consumption, and short analysis time for single sample(<15 min). The results were proved to be credible by high performance liquid chromatographyàmass spectrometry(LC-MS) and electrospray ionization mass spectrometry, respectively. Moreover, the limitation standard for the toxic aconitines in 20 APCMs was established based on the holistic weight toxicity(HWT) evaluation and the Chinese Pharmacopoeia severally, and turned out that HWT-based toxicity evaluation results were closer to the real clinical applications. Hence,a more accurate and reliable APCM toxicity limitation was established and expected to play an important guiding role in clinics. The current study extended the power of ambient MS as a method for the direct quantification of molecules in complex samples, which is commonly required in pharmaceutical analysis,food safety control, public security, and many other disciplines.