Homoisoflavonoids profiling of Ophiopogon japonicus by off‐line coupling high‐speed countercurrent chromatography with high‐performance liquid chromatography–diode array detector‒quadrupole time‐of‐flight tandem mass spectrometry

Abstract

Roots of Ophiopogon japonicus have been used as a functional food ingredient and traditional Chinese medicine for a long time in China. Homoisoflavonoids are one of the major kinds of bioactive compounds in O. japonicus; however, literature data about its homoisoflavonoids profile are scarce because of the complex ingredients with low abundance. Here, homoisoflavonoid fraction was prepared by petroleum ether extraction. Then, a high-speed countercurrent chromatography offline coupling with high-performance liquid chromatography-diode array detectorquadrupole time-of-flight tandem mass spectrometry was developed for systematic identification of homoisoflavonoids. After that, 39 homoisoflavonoids, including 29 homoisoflavanone and 10 homoisoflavone, were unambiguously or tentatively identified, while 12 of them were reported in O. japonicus for the first time. Finally, eight available homoisoflavonoids were sensitively, precisely, and accurately determined by standard calibration curves, with limit of detection and limit of quantification in the range of 0.05-0.30 μg/mL and 0.12-0.66 μg/mL, relative standard deviation less than 7.3% for intra-and interday variations, and recovery at 94.5-105.2%. Collectively, our developed method is efficient, reliable, and valuable to profile chemical components of complex natural products.

Characterization and Discrimination of Ophiopogonis Radix with Different Levels of Sulfur Fumigation Based on UPLC-QTOF-MS Combined Molecular Networking with Multivariate Statistical Analysis

“…The type I homoisoflavonoids fragmentation behavior was also observed in Peak 83 . Peak 83 showed [M-H] − ion at m/z 327.1245 and generated fragments ions at m/z 206.0581([M-H-B-ring-CH 2 ] − ), which is the same as that reported in the literature [ 46 ]. In addition, the [(M-H-B-ring-CH 2 -CO] − product ion was observed at m/z 178.0637.…”

The challenge of separating and determining biologically active electrostatically stabilized silanates using the high‐performance liquid chromatography technique

“…This resulted in the shorter retention times and affected the obtained selectivity results for the analyzed ES-silanates, which were significantly better when using the acetonitrile/water mixture (Table 2ac). Satisfactory separation selectivity is often achieved by either changing the composition of the mobile phase or the type of organic eluent, which has a direct impact on the solvation process [41][42][43][44].…”

Diagnostic ion filtering targeted screening and isolation of anti‐inflammatory iridoid glycosides from Hedyotis diffusa

“…Then, the guard column was connected to the six‐port switching valve instead of sample loop. Two‐phase solvent systems suitable for HSCCC were optimized according to the partition coefficient (K) values of target compounds [10]. Different volume ratios of ethyl acetate/ n ‐butanol/water (1 mL) and 1.0 mg of ground H. diffusa were thoroughly mixed.…”