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A Dilute-and-Shoot Based UPLC-MS/MS Method for Multimycotoxins Analysis in Astragali radix

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Background: Astragali radix is prone to be contaminated by various mycotoxins, leading to unpredictable threats on the quality and safety of Astragali radix and the health of the consumers. Therefore, the determination of multimycotoxins is imperative. Objective: To develop an efficient, sensitive, fast, and multianalyte method for detecting multimycotoxins in Astragali radix. Methods: A selective dilute-and-shoot pretreatment procedure based ultra-performance LC–tandem MS (UPLC-MS/MS) method was developed for sensitive determination of multimycotoxins in Astragali radix, including aflatoxin (AF) B1, B2, G1, G2, and ochratoxin A. The five mycotoxins were extracted by the dilute-and-shoot pretreatment procedure followed by UPLC-MS/MS detection. Types of sample extraction solvent, mobile-phase compositions and MS/MS parameters, and dilute-and-shoot conditions were optimized. Results: The optimized chromatographic and mass spectrometric conditions allowed the separation and detection of the five mycotoxins within 5 min. The validated UPLC-MS/MS method exhibited good sensitivity with LOD and LOQ lower than 0.2 and 0.5 μg/kg, respectively. RSD values for method precision were lower than 9%. Recoveries obtained were between 90.87 and 108.44% for all the analytes with RSDs of 3.96–8.03%. The developed method was applied for the detection of the 5 mycotoxins in 18 batches of Astragali radix with good determination performance and no matrix interferences. Two samples collected from Shanxi province and Neimenggu Autonomous Region in China were positive for AFB1 at 3.24 and 2.69 μg/kg, respectively. Conclusions: The dilute-and-shoot procedure allowed for the extraction of the mycotoxins with advantages of simple pretreatment, small extraction time, high selectivity and accuracy, as well as being cost effective and easy to operate without any clean-up steps. Highlights: This is the first report on dilute-and-shoot approach for mycotoxins extraction and detection in Chinese medicinal material matrixes.
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Document Type: Research Article

Affiliations: Capital Medical University, Beijing Friendship Hospital, Department of Traditional Chinese Medicine, 95 Yong’an Rd, Beijing 100050, China

Publication date: July 1, 2019

This article was made available online on January 4, 2019 as a Fast Track article with title: "A Dilute-and-Shoot Based UPLC-MS/MS Method for Multimycotoxins Analysis in Astragali radix".

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  • The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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