LC/UV(PDA)およびLC/TOF-MSによる液状調味料中シクロピアゾン酸の分析法開発とその妥当性確認

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  • Development of analytical method for cyclopiazonic acid in liquid seasoning by LC/UV(PDA) and LC/TOF-MS, and its validation study
  • LC/UV(PDA)オヨビ LC/TOF-MS ニ ヨル エキジョウ チョウミリョウ チュウ シクロピアゾンサン ノ ブンセキホウ カイハツ ト ソノ ダトウセイ カクニン

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A simple, rapid, and precise method for the determination of cyclopiazonic acid (CPA) in liquid seasoning was developed, which uses liquid chromatography with ultraviolet and photodiode array detection LC/UV(PDA) and liquid chromatography with time-of-flight mass spectrometry (LC/TOF-MS). CPA in liquid seasoning was subjected to ethyl acetate extraction, and solid-phase extraction using Oasis® HLB. LC/UV(PDA) was used for qualitative and quantitative analysis, and LC/TOF-MS was used as the confirmatory method. The limit of detection (S/N = 3) and the limit of quantification (S/N > 10) of CPA in LC/UV(PDA) were 0.01 μg/mL and 0.03 μg/mL, respectively. Standard materials were prepared for quality control samples (a low concentration of 0.2 μg/mL and a high concentration of 2.0 μg/mL), and internal quality control was performed. As a result, the trueness of the low concentration sample and the high concentration samples was 80.3% and 81.6%, respectively. The relative standard deviation (RSD) of repeatability was 5.3% or less, whereas that of intermediate precision was less than 10.1%. The results suggest that the developed method is useful for the determination of CPA in liquid seasoning.

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