Objective: To establish a high-performance liquid chromatography (HPLC) coupled with electrospray ionization (ESI) tandem triple quadrupole mass spectrometry (QQQ/MS) method for the simultaneous determination of multiple residues of ten mycotoxins (fumonisin B1, fumonisin B2, fumonisin B3, aflatoxin G1, aflatoxin G2, aflatoxin B1, aflatoxin B2, T-2 toxin, ochratoxin A and zearalenone) in Polygonati Rhizoma and Ophiopogonis Radix by solid-phase extraction. Methods: Samples were extracted with 70% methanol solution by vortex and oscillation. The concentrated liquid supernatant was purified by a hydrophilic-lipophilic balance (HLB) solid-phase extraction (SPE) column. HPLC separation was performed on an Agilent Eclipse plus C18 column. 0.01% formic acid (containing 0.5 mmol·L-1 ammonium acetate) and acetonitrile-methanol (50∶50) solution was used as mobile phase in positive mode. 0.1% acetic acid-acetonitrile was used as the mobile phase in negative mode. MS/MS was adopted for multiple reaction monitoring (MRM) in the positive/negative mode. The quantification was achieved using matrix-matched standard calibrations as the external standard. Results: Under the optimized conditions, the calibration curve showed good linearity with correlation coefficients above 0.99. The limits of detection (LODs) were 0.20-4.0 μg·kg-1(Ophiopogonis Radix) and 0.33-0.67 μg·kg-1 (Polygonati Rhizoma). The recoveries of 10 mycotoxins at three levels were in the range of 72.3%-130.8%(Ophiopogonis Radix)and 69.7%-122.7%(Polygonati Rhizoma),and the relative standard deviation(RSDs) were 0.50%-7.7%(Ophiopogonis Radix)and 0.13%-8.7% (Polygonati Rhizoma). The result showed that among 14 batch of Polygonati Rhizoma samples, zearalenone was detected in one batch of sample, with a detection value of 1.48 μg·kg-1 and the detection rate of 5.0%. Amang 20 batches of Ophiopogonis Radix samples, fumonisin B2 were detected in 14 batches of samples, with a detection value of 4.99-378.99 μg·kg-1 and the detection rate of 70.0%. Conclusion: This experiment provides a simple, rapid, and practical method that is suitable for the quantitative analysis of 10 kinds of fungal mycotoxin in Ophiopogonis Radix and Polygonati Rhizoma. Some mycotoxin residues in Ophiopogonis Radix and Polygonati Rhizoma have certain health risks and should arouse our attention more.
SHEN Li, TANG Yan, CHEN Tie-zhu, CUI Hong-mei, LUO Hen
. Determination of 10 mycotoxins in Polygonati Rhizoma and Ophiopogonis Radix as a genuine regional drug of Sichuan by solid-phase extraction coupled with LC-MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2023
, 43(8)
: 1369
-1380
.
DOI: 10.16155/j.0254-1793.2023.08.13
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