Rapid and reliable determination of illegal adulterant in herbal medicines and dietary supplements by LC/MS/MS.

摘要

In recent years, dietary supplements and herbal medicines are increasing in popularity all over the world. However, it is problematic that some manufacturers illegally included synthetic drugs in their products. Due to the extremely complex matrices of those products, most existing methods for screening illegal adulterations are time-consuming and liable to false positive. In this paper, a robust LC/MS/MS method for the high-throughput, sensitive and reliable determination of illegal adulterations from herbal medicines and dietary supplements was established. Minimal LC separation was employed and MRM was used to simultaneously monitor the three transitions under their respective optimal collision energy for each compound. Positive results were determined only if well-defined peaks appeared at all of the three transitions and the ratios among the peak areas were within given threshold. In this study, the method had been applied for the screening of nine most commonly adulterated therapeutic substances,such as sildenafil (Viagra) and famotidine, and the lower limits of detection of these compounds ranged from 0.05 to 1.5 ng/ml. Little sample preparation was needed for this method and the analysis time was less than 5 min/sample. The reliability has been demonstrated by the test with blank matrix. Over 200 products that were under suspicion by SDA of China had been assayed and till now no false negative or positive result was found. This method is rapid, simple, reliable and capable of screening multiple adulterants in one run.