title: Rapid and sensitive determination of phytosterols in functional foods and medicinal herbs by using UHPLC-MS/MS with microwave-assisted derivatization combined with dual ultrasound-assisted dispersive liquid-liquid microextraction.
abstract: In this work, a hyphenated technique of dual ultrasound-assisted dispersive liquid-liquid microextraction combined with microwave-assisted derivatization followed by ultra high performance liquid chromatography tandem mass spectrometry has been developed for the determination of phytosterols in functional foods and medicinal herbs. Multiple reaction monitoring mode was used for the tandem mass spectrometry detection. A mass spectrometry sensitive reagent, 4'-carboxy-substituted rosamine, has been used as the derivatization reagent for five phytosterols, and internal standard diosgenin was used for the first time. Parameters for the dual microextraction, microwave-assisted derivatization, and ultra high performance liquid chromatography tandem mass spectrometry were all optimized in detail. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect, extremely low limits of detection (0.005-0.015 ng/mL) and limits of quantification (0.030-0.10 ng/mL) were achieved. The proposed method was compared with previously reported methods. It showed better sensitivity, selectivity, and accuracy. The matrix effect was also significantly reduced. The proposed method was successfully applied to the determination of five phytosterols in vegetable oil (sunflower oil, olive oil, corn oil, peanut oil), milk and orange juice (soymilk, peanut milk, orange juice), and medicinal herbs (Ginseng, Ganoderma lucidum, Cordyceps, Polygonum multiflorum) for the quality control of functional foods and medicinal herbs.
authors.affiliation: Key Laboratory of Tibetan Medicine Research and Qinghai Key Laboratory of Qinghai-Tibet Plateau Biological Resources, Northwest Institute of Plateau Biology, Chinese Academy of Science, Xining, Qinghai, P.R. China.
authors.forename: Jing
authors.initials: J
authors.lastname: Sun
authors.affiliation: Key Laboratory of Tibetan Medicine Research and Qinghai Key Laboratory of Qinghai-Tibet Plateau Biological Resources, Northwest Institute of Plateau Biology, Chinese Academy of Science, Xining, Qinghai, P.R. China.|Shandong Provincial Key Laboratory of Life-Organic Analysis and Key Laboratory of Pharmaceutical Intermediates and Analysis of Natural Medicine, College of Chemistry and Chemical Engineering, Qufu Normal University, Qufu, Shandong, P. R. China.
authors.forename: Xian-En
authors.initials: XE
authors.lastname: Zhao
authors.affiliation: Key Laboratory of Tibetan Medicine Research and Qinghai Key Laboratory of Qinghai-Tibet Plateau Biological Resources, Northwest Institute of Plateau Biology, Chinese Academy of Science, Xining, Qinghai, P.R. China.
authors.forename: Jun
authors.initials: J
authors.lastname: Dang
authors.affiliation: Shandong Provincial Key Laboratory of Life-Organic Analysis and Key Laboratory of Pharmaceutical Intermediates and Analysis of Natural Medicine, College of Chemistry and Chemical Engineering, Qufu Normal University, Qufu, Shandong, P. R. China.
authors.forename: Xiaoyan
authors.initials: X
authors.lastname: Sun
authors.affiliation: Shandong Provincial Key Laboratory of Life-Organic Analysis and Key Laboratory of Pharmaceutical Intermediates and Analysis of Natural Medicine, College of Chemistry and Chemical Engineering, Qufu Normal University, Qufu, Shandong, P. R. China.
authors.forename: Longfang
authors.initials: L
authors.lastname: Zheng
authors.affiliation: Shandong Provincial Key Laboratory of Life-Organic Analysis and Key Laboratory of Pharmaceutical Intermediates and Analysis of Natural Medicine, College of Chemistry and Chemical Engineering, Qufu Normal University, Qufu, Shandong, P. R. China.
authors.forename: Jinmao
authors.initials: J
authors.lastname: You
authors.affiliation: Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan, Shandong, China.
authors.forename: Xiao
authors.initials: X
authors.lastname: Wang
mesh_terms: D002623:Chemistry Techniques, Analytical / Q000379:methods*; D002851:Chromatography, High Pressure Liquid; D005504:Food Analysis; D055951:Functional Food / Q000032:analysis*; D057230:Limit of Detection; D059627:Liquid Phase Microextraction; D008872:Microwaves; D010840:Phytosterols / Q000032:analysis*; D010946:Plants, Medicinal / Q000737:chemistry*; D053719:Tandem Mass Spectrometry
chemical_list: D010840:Phytosterols
keywords: derivatization; dispersive liquid-liquid microextraction; phytosterol; sensitivity enhancement; triple quadrupole mass spectrometry