A novel pretreatment method ionic liquid-based dispersive liquid-liquid followed high-performance liquid chromatography was established and applied in the analysis of Silychristin, Silydianin, Silybin ,Silybin B, Isosilybin A, Isosilybin B in silbbum marianum. The critical parameters affecting dispersive liquid-liquid micro-extraction (DLLME), including selection of dispersive solvent and extraction solvent, volume of dispersive solvent and extraction solvent, adjustment of pH, salt concentration, extraction time, were investigated by single factor study. Under optimum conditions, all of the target analytes presented good linearity (r > 0.9991) and satisfied recoveries (Recoveries > 89.5%, relative standard deviation (RSD) < 4.6%). The limits of detection and quantification were 0.16 to 0.74 ng kg− 1 and 0.42 to 2.52 ng kg− 1, respectively. The developed method is sensitive, rapid, accurate and employable to simultaneously determine six target compounds in silbbum marianum.
For determination of cholesterol, cholestanol, rapeseed sterol, ergosterol, rapeseed sterol, stigmasterol-sitosterol, and stigmasterol in rapeseed, an accelerated solvent extraction followed gas chromatography-tandem mass spectrometry technique was developed. The sterols were isolated after derivatization and identified using accelerated solvent extraction coupled with gas chromatography-mass spectrometry (GC-MS/MS). The results revealed a good linear relationship between the peak area and the corresponding mass concentration of the eight sterols in the range of 2-1000 mg/L, with correlation coefficients all greater than 0.9991, detection limits of 1.12–1.61 mg/kg, and quantification limits of 3.73–5.41 mg/kg, spiked recovery determination ranging from 5 to 20 mg/kg.The average recoveries were 89.5-105.2% at mg/kg supplemental level, and the precision was lower than 5.0%. The developed method was efficient, simple and accurate, and suitable for qualitative and quantitative analysis of eight sterol compounds in rapeseed, providing a method for rapid determination of sterol compounds in rapeseed.
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