PMID- 34227338 OWN - NLM STAT- MEDLINE DCOM- 20210727 LR - 20220915 IS - 1872-2059 (Electronic) IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 39 IP - 5 DP - 2021 May TI - [Design and application of special solid phase extraction column for three cannabinol compounds in hemp]. PG - 534-540 LID - 10.3724/SP.J.1123.2020.09025 [doi] AB - Cannabidiol (CBD), cannabinol (CBN), and Delta9-tetrahydrocannabinol (THC) are the most important components of hemp, whose concentrations determine the properties and applications of hemp. Hemp contains a large number of impurities, which must be removed from the extracting solution before determining the cannabinol contents by ultra-high performance liquid chromatography (UHPLC). Neutral alumina, magnesium silicate, and graphitized carbon black have different surface characteristics when used as adsorbents. The removal rates of pigments, total sugar, total fatty acid glyceride, and metal ions as well as the recoveries of the three cannabinols in the extraction solution were evaluated. The amounts of neutral alumina, magnesium silicate, and graphitized carbon black were 1.80 g, 0.15 g, and 0.05 g, respectively. The three adsorbents were mixed well and packed into a polypropylene pipe to prepare a special 2 g/6 mL solid phase extraction (SPE) column for determining the three cannabinol compounds in hemp. The chemical components of the hemp flowers and leaves were extracted with an ethyl acetate/methanol (9ratio1, v/v) mixture. After the extracting solution was allowed to pass through the SPE column, the recoveries of CBD, CBN, and Delta9-THC were 98.9%, 95.7%, and 99.2%, respectively. The removal rates of xanthophyll, chlorophyll a, and chlorophyll were 96.3%, 99.2%, and 95.5%, respectively. The removal rates of total sugar, total fatty glyceride, and metal ions were 98.5%, 96.9%, and 85.4%, respectively. In this study, the chromatographic conditions for analyzing the three cannabinol compounds were optimized. The cannabinol compounds were separated within 10 min on an Eclipse Plus C18 column (50 mmx2.1 mm, 1.8 mum) using a mobile phase consisting of 1% (v/v) acetic acid and acetonitrile (30ratio70, v/v) at a flow rate of 0.5 mL/min. The detection wavelength was set at 210 nm with a diode array detector, and the sample injection volume was 1 muL. Good linear relationships were observed between the mass peak areas and mass concentrations of CBD, CBN, and Delta9-THC in the range of 0.5-50 mg/L. The corresponding correlation coefficients (R(2)) were 0.9983, 0.9995, and 0.9981, while the detection limits were 0.45 mug/L, 0.53 mug/L, and 0.38 mug/L. The recoveries of CBD, CBN, and Delta9-THC were 90.3%-96.9%, 93.7%-95.6%, and 90.8%-96.1%, with relative standard deviations (RSDs) of 2.2%-6.1%, 4.1%-8.0%, and 2.4%-4.8%, respectively. The results were satisfactory, demonstrating that the special SPE column made of neutral alumina, magnesium silicate, and graphitized carbon black was well suited for the determination of the three cannabinol compounds in hemp. FAU - Shen, Shuchang AU - Shen S AD - Center of Analytical and Testing, Qiqihar University, Qiqihar 161006, China. FAU - Li, Shaohua AU - Li S AD - Center of Analytical and Testing, Qiqihar University, Qiqihar 161006, China. FAU - Guo, Li AU - Guo L AD - Daqing Branches of Heilongjiang Academy of Agricutural Sciences, Daqing 163316, China. FAU - Lu, Weichao AU - Lu W AD - Center of Analytical and Testing, Qiqihar University, Qiqihar 161006, China. FAU - Li, Qiushi AU - Li Q AD - Center of Analytical and Testing, Qiqihar University, Qiqihar 161006, China. LA - chi PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 19GBJ60SN5 (Cannabidiol) RN - 7J8897W37S (Dronabinol) RN - 7UYP6MC9GH (Cannabinol) SB - IM MH - *Cannabidiol/isolation & purification MH - Cannabinol/*isolation & purification MH - *Cannabis/chemistry MH - Dronabinol/*isolation & purification MH - Solid Phase Extraction PMC - PMC9404009 OTO - NOTNLM OT - cannabidiol OT - cannabinol OT - hemp OT - special solid phase extraction column OT - ultra-high performance liquid chromatography (UHPLC) OT - Delta9-tetrahydrocannabinol; EDAT- 2021/07/07 06:00 MHDA- 2021/07/28 06:00 PMCR- 2021/05/08 CRDT- 2021/07/06 07:00 PHST- 2021/07/06 07:00 [entrez] PHST- 2021/07/07 06:00 [pubmed] PHST- 2021/07/28 06:00 [medline] PHST- 2021/05/08 00:00 [pmc-release] AID - 1000-8713-39-5-534 [pii] AID - 10.3724/SP.J.1123.2020.09025 [doi] PST - ppublish SO - Se Pu. 2021 May;39(5):534-540. doi: 10.3724/SP.J.1123.2020.09025.