Identification and determination of chemical constituents of Citrus reticulata semen through ultra high performance liquid chromatography combined with Q Exactive Orbitrap tandem mass spectrometry

Abstract

Citrus reticulata semen, a traditional Chinese medicinal material, has desirable medicinal and dietary properties. In this study, a method combining ultra high performance liquid chromatography with Q Exactive Orbitrap tandem mass spectrometry was established and validated for the identification and analysis of the chemical components of C. reticulata semen for the first time. The evaluation of different retention times and fragmentation characteristics, as well as comparative analysis with the literature, resulted in the identification of 35 chemical constituents, including 21 flavonoids and 14 other compounds. The 21 flavonoids derived from C. reticulata semen were reported for the first time. Seven of the chemical components of C. reticulata semen were quantitatively analyzed using the developed method under the optimal conditions. The results showed that the content of limonin, hesperidin, nobiletin, synephrine, tangeretin, 3,5,6,7,8,3′,4′‐heptamethoxyflavone and 5‐hydroxide‐6,7,8,3′,4′‐pentamethoxyflavone in C. reticulata semen was 11.1666, 0.0404, 0.0092, 0.0255, 0.0087, 0.0010, and 0.0008 mg/g, respectively. This study demonstrated that the ultra high performance liquid chromatography Q Exactive Orbitrap mass spectrometry based method can be used to rapidly and reliably analyze the chemical constituents of C. reticulata semen. These results provide a scientific basis for further studies of C. reticulata semen.

In vitro human intestinal microbiota biotransformation of nobiletin using liquid chromatography–mass spectrometry analysis and background subtraction strategy

“…The product ion at m/z 197.0073 was formed from ion at m/z 389.1221 by the RDA cleavage. Based on the retention time, MS 2 fragment ions and previous report [11, 15], metabolite 3 was identified as 5‐demethylnobiletin (5‐hydroxy‐6,7,8,3′,4′‐pentamethoxyflavone) (Figure 3D). The MS fragmentation pathways of parent compound and three metabolites are shown in Supporting Information Figure S2.…”

“…Compared with the structure of metabolite 1 and 3, metabolite 2 could be reasonably characterized as 5-hydroxy-6,7,3′,4′-tetramethoxyflavone [12]. [11,15], metabolite 3 was identified as 5-demethylnobiletin (5-hydroxy-6,7,8,3′,4′pentamethoxyflavone) (Figure 3D). The MS fragmentation pathways of parent compound and three metabolites are shown in Supporting Information Figure S2.…”

Identification of lipophilic components in Citri Reticulatae Pericarpium cultivars by supercritical CO2 fluid extraction with ultra‐high‐performance liquid chromatography–Q Exactive Orbitrap tandem mass spectrometry

“…Compound 2 produced a quasi‐molecular [M+H] + peak at m/z 124.0394 and further fragmentations at m/z 96.0447 [M+H‐CO] + , 80.0504 [M+H‐CO 2 ] + , 78.0345 [M‐COOH] + , and 53.0393 [M+H‐COOH‐C 2 H 3 ] + . By comparison with the relative literature [19], compound 2 was confirmed as nicotinic acid.…”

Fingerprint Analysis of Phenolic Acid Extract of Salvia Miltiorrhiza by Digital Reference Standard Analyzer With One or Two Reference Standards

“…Therefore, ensuring the e cient and safe use of TCM is an important issue. Given the complex components of TCMs, it is crucial to carry out a holistic quality control methodology, involving ngerprint technology and multi-components determination technology [1][2][3][4]. However, these technologies cannot be realized without reference standard (RS), which has brought great pressure to both providers and users.…”