Quantification of atractyloside in Fructus Xanthii using HILIC-ESI-MS/MS

Fructus Xanthii is thought to be toxic in traditional Chinese medicine. The bur is usually taken orally to treat certain diseases, as accordingly results in poisoning incidents happen occasionally in China. Atractyloside, a highly hydrophilic compound, is the main lethal component in Fructus Xanthii. Unfortunately, so far the quantitative method of this toxic compound is unavailable in Chinese Pharmacopoeia. In this study, a simple and rapid method using hydrophilic interaction liquid chromatography-tandem mass spectrometry has been developed to quantify the toxic component in Fructus Xanthii. The method was further validated from linearity, sensitivity, accuracy, and precision and extraction efficiency. As a result, the limits of detection and quantification were 0.0625 and 0.25ng/mL, respectively, and the accuracy ranged from 99.37 to 103.97% with relative standard deviation less than 4.86%. The established method was then used to determine the toxin contained in 28 batches of commercial herbal drugs, as showed that the method was satisfying for determination of atractyloside contained in these samples over a large content range of 0.19 to 80.75mg/g, which, together with time-saving, sensitive and accurate characteristics, makes this method very attractive for quantitative analysis of the toxic component in the crude drug and related Chinese medicine preparations.