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The dried ripe fruits of Xanthium sibiricum (Cang'erzi) are used in traditional Chinese medicine for the treatment of nasal congestion, nasal discharge, allergic rhinitis, sinusitis, and wind-cold headaches. Carboxyatractyloside and atractyloside are important constituents of the fruits because these diterpenoid glycosides are responsible for their toxicity. In order to evaluate procedures for reducing the amount of the more toxic carboxyatractyloside, the fruits were dried and heated with different methods. Carboxyatractyloside and atractyloside were analysed by a new reversed-phase high-performance liquid chromatographic method using liquid chromatography-diode array detector-tandem mass spectrometry analysis. The results revealed that temperature and drying methods have a strong influence on the content of carboxyatractyloside and atractyloside. Fruits which were treated at higher temperatures showed a lower content of carboxyatractyloside and an increased content of atractyloside, which is 50 times less toxic. This indicates that the roasting process can reduce toxicity effectively. The microbiological colonisation of Xanthium fruits is also reduced by roasting and by drying above 100 °C. For the safe use of Cang'erzi, the effect of processing should be monitored and analysis of carboxyatractyloside and atractyloside should be obligatory in quality control., (Georg Thieme Verlag KG Stuttgart · New York.)