Lovastatin in lactone and hydroxy acid forms and citrinin in red yeast rice powders analyzed by HPTLC-UV/FLD
Lovastatin in lactone and hydroxy acid forms and citrinin in red yeast rice powders analyzed by HPTLC-UV/FLD
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DOI：
10.1007/s00216-019-02039-y
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发表时间：
2019-10-01
影响因子：
4.3
通讯作者：
Morlock, Gertrud E.
中科院分区：
文献类型：
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作者：
Klingelhoefer, Ines;Morlock, Gertrud E.
针对富含色素的红曲米制品，建立了一种快速定量的高效薄层色谱（HPTLC）分析方法。本文分析了19种红曲产品（包括红曲粉、膳食补充剂和中成药（血脂康和脂必妥））中的活性成分洛伐他汀（以内酯（LL）和羟基酸形式（LH）存在）以及真菌毒素桔霉素。包括样品制备在内的HPTLC方法可以高通量地处理富含基质的样品（每次分析10分钟），并且具有极高的成本效益（每次分析的运行成本为0.5欧元）。对于快速方案，选择高达10 μ L的施用体积，尽管更高的施用体积仍将降低LOD，LL和LH的LOD为30 mg/kg，桔霉素的LOD为4 mg/kg。由于采用了最低限度的样品制备，总体平均回收率良好（109.9% +/- 5.9%;在3个加标水平下重复测量每份新鲜样品制备液中的3种分析物）。在红曲米基质中重复校准（每种分析物5次）显示出非常令人满意的决定系数（>= 0.9991;平均值0.9996）。对于三种浓度水平的三种分析物，在整个程序（包括样品制备）中分析的红曲基质中获得的平均中间精密度非常令人满意（
For the analysis of pigment-rich red yeast rice products, a fast quantitative high-performance thin-layer chromatography (HPTLC) method was newly developed and validated. The active ingredient lovastatin, present in lactone (LL) and hydroxy acid forms (LH), as well as the mycotoxin citrinin were analyzed in 19 red yeast rice products, including powders, dietary supplements, and Chinese proprietary medicines (Xuezhikang and Zhibituo). The HPTLC method including sample preparation allows a high throughput of matrix-rich samples (10 min per analysis) and is highly cost-efficient (running costs of 0.5 Euro per analysis). For a fast protocol, application volumes up to 10 mu L were selected although higher application volumes will lower still the LODs, which were 30 mg/kg for LL and LH as well as 4 mg/kg for citrinin. Thanks to the minimalistic sample preparation, the overall mean recovery rate was good (109.9% +/- 5.9%; repeated measurements of the three analytes per fresh sample preparation at three spike levels). Repeated calibrations (five per analyte) in the red yeast rice matrix showed highly satisfying determination coefficients (>= 0.9991; mean 0.9996). For three analytes at three concentration levels, the obtained mean intermediate precisions in red yeast rice matrix analyzed over the whole procedure including sample preparation were highly satisfying (