{"title":"利用 1H NMR 定量分析黄芩根茎中的苯丁酸类化合物通过定量 1H NMR.","authors":"Boonwiset Seaho, Chatkamon Lekwongphaiboon, Ngampuk Tayana, Wichayasith Inthakusol, Sumet Kongkiatpaiboon, Wiratchanee Mahavorasirikul, Saisuree Prateeptongkum, Nongnaphat Duangdee","doi":"10.1002/pca.3475","DOIUrl":null,"url":null,"abstract":"<p><strong>Introduction: </strong>Quantitative determination of pharmacologically active constituents in medicinal plants is critical for quality control. Due to the chemical complexity of the crude plant extracts, the presence of interfering compounds is often problematic for the unambiguous quantitation of the designed bioactive compounds. Considering the method of quantification, quantitative NMR spectroscopy (qNMR) has gained substantial popularity as a powerful and effective technique for both qualitative and quantitative analyses of natural products.</p><p><strong>Objective: </strong>The aim of this study is to develop a quantitative NMR method for quantifying the bioactive phenylbutanoids in Zingiber cassumunar rhizome crude extract.</p><p><strong>Methods: </strong>Quantitative <sup>1</sup>H NMR (qHNMR) measurements were performed on a 600 MHz NMR spectrometer using an internal standard for the determination of the absolute quantities of four phenylbutanoids in Z. cassumunar rhizome crude extract.</p><p><strong>Results: </strong>The direct quantification of four characteristic phenylbutanoids, i.e., (E)-1-(3',4'-dimethoxyphenyl)butadiene (DMPBD), (E)-1-(2',4',5'-trimethoxyphenyl)butadiene (TMPBD), (E)-4-(3',4'-dimethoxyphenyl)but-3-en-1-ol, and (E)-4-(3',4'-dimethoxyphenyl)but-3-en-1-yl acetate, in crude extract by qHNMR using an internal standard was achieved, with high specificity and sensitivity. The selected <sup>1</sup>H NMR signals could unambiguously be assigned and did not overlap with other resonances, including the highly similar compounds DMPBD and TMPBD. The method is linear in the concentration range of 0.70-14.52 mg/mL, with a limit of quantification of 0.46-0.68 mg/mL. The RSD values of intraday and interday precisions are in the range of 0.23%-0.74% and 0.29%-0.52%, respectively. The average recoveries are 99.54%-100.18%.</p><p><strong>Conclusions: </strong>A rapid, accurate, and precise method using <sup>1</sup>H NMR for the simultaneous quantitation of four phenylbutanoids in the crude extract of Z. cassumunar rhizome was developed and validated.</p>","PeriodicalId":20095,"journal":{"name":"Phytochemical Analysis","volume":" ","pages":""},"PeriodicalIF":3.0000,"publicationDate":"2024-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Absolute Quantification of Phenylbutanoids in Zingiber cassumunar Roxb. Rhizome by Quantitative <sup>1</sup>H NMR.\",\"authors\":\"Boonwiset Seaho, Chatkamon Lekwongphaiboon, Ngampuk Tayana, Wichayasith Inthakusol, Sumet Kongkiatpaiboon, Wiratchanee Mahavorasirikul, Saisuree Prateeptongkum, Nongnaphat Duangdee\",\"doi\":\"10.1002/pca.3475\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><strong>Introduction: </strong>Quantitative determination of pharmacologically active constituents in medicinal plants is critical for quality control. Due to the chemical complexity of the crude plant extracts, the presence of interfering compounds is often problematic for the unambiguous quantitation of the designed bioactive compounds. Considering the method of quantification, quantitative NMR spectroscopy (qNMR) has gained substantial popularity as a powerful and effective technique for both qualitative and quantitative analyses of natural products.</p><p><strong>Objective: </strong>The aim of this study is to develop a quantitative NMR method for quantifying the bioactive phenylbutanoids in Zingiber cassumunar rhizome crude extract.</p><p><strong>Methods: </strong>Quantitative <sup>1</sup>H NMR (qHNMR) measurements were performed on a 600 MHz NMR spectrometer using an internal standard for the determination of the absolute quantities of four phenylbutanoids in Z. cassumunar rhizome crude extract.</p><p><strong>Results: </strong>The direct quantification of four characteristic phenylbutanoids, i.e., (E)-1-(3',4'-dimethoxyphenyl)butadiene (DMPBD), (E)-1-(2',4',5'-trimethoxyphenyl)butadiene (TMPBD), (E)-4-(3',4'-dimethoxyphenyl)but-3-en-1-ol, and (E)-4-(3',4'-dimethoxyphenyl)but-3-en-1-yl acetate, in crude extract by qHNMR using an internal standard was achieved, with high specificity and sensitivity. The selected <sup>1</sup>H NMR signals could unambiguously be assigned and did not overlap with other resonances, including the highly similar compounds DMPBD and TMPBD. The method is linear in the concentration range of 0.70-14.52 mg/mL, with a limit of quantification of 0.46-0.68 mg/mL. The RSD values of intraday and interday precisions are in the range of 0.23%-0.74% and 0.29%-0.52%, respectively. The average recoveries are 99.54%-100.18%.</p><p><strong>Conclusions: </strong>A rapid, accurate, and precise method using <sup>1</sup>H NMR for the simultaneous quantitation of four phenylbutanoids in the crude extract of Z. cassumunar rhizome was developed and validated.</p>\",\"PeriodicalId\":20095,\"journal\":{\"name\":\"Phytochemical Analysis\",\"volume\":\" \",\"pages\":\"\"},\"PeriodicalIF\":3.0000,\"publicationDate\":\"2024-11-04\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Phytochemical Analysis\",\"FirstCategoryId\":\"99\",\"ListUrlMain\":\"https://doi.org/10.1002/pca.3475\",\"RegionNum\":3,\"RegionCategory\":\"生物学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"BIOCHEMICAL RESEARCH METHODS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Phytochemical Analysis","FirstCategoryId":"99","ListUrlMain":"https://doi.org/10.1002/pca.3475","RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}
Absolute Quantification of Phenylbutanoids in Zingiber cassumunar Roxb. Rhizome by Quantitative 1H NMR.
Introduction: Quantitative determination of pharmacologically active constituents in medicinal plants is critical for quality control. Due to the chemical complexity of the crude plant extracts, the presence of interfering compounds is often problematic for the unambiguous quantitation of the designed bioactive compounds. Considering the method of quantification, quantitative NMR spectroscopy (qNMR) has gained substantial popularity as a powerful and effective technique for both qualitative and quantitative analyses of natural products.
Objective: The aim of this study is to develop a quantitative NMR method for quantifying the bioactive phenylbutanoids in Zingiber cassumunar rhizome crude extract.
Methods: Quantitative 1H NMR (qHNMR) measurements were performed on a 600 MHz NMR spectrometer using an internal standard for the determination of the absolute quantities of four phenylbutanoids in Z. cassumunar rhizome crude extract.
Results: The direct quantification of four characteristic phenylbutanoids, i.e., (E)-1-(3',4'-dimethoxyphenyl)butadiene (DMPBD), (E)-1-(2',4',5'-trimethoxyphenyl)butadiene (TMPBD), (E)-4-(3',4'-dimethoxyphenyl)but-3-en-1-ol, and (E)-4-(3',4'-dimethoxyphenyl)but-3-en-1-yl acetate, in crude extract by qHNMR using an internal standard was achieved, with high specificity and sensitivity. The selected 1H NMR signals could unambiguously be assigned and did not overlap with other resonances, including the highly similar compounds DMPBD and TMPBD. The method is linear in the concentration range of 0.70-14.52 mg/mL, with a limit of quantification of 0.46-0.68 mg/mL. The RSD values of intraday and interday precisions are in the range of 0.23%-0.74% and 0.29%-0.52%, respectively. The average recoveries are 99.54%-100.18%.
Conclusions: A rapid, accurate, and precise method using 1H NMR for the simultaneous quantitation of four phenylbutanoids in the crude extract of Z. cassumunar rhizome was developed and validated.
期刊介绍：
Phytochemical Analysis is devoted to the publication of original articles concerning the development, improvement, validation and/or extension of application of analytical methodology in the plant sciences. The spectrum of coverage is broad, encompassing methods and techniques relevant to the detection (including bio-screening), extraction, separation, purification, identification and quantification of compounds in plant biochemistry, plant cellular and molecular biology, plant biotechnology, the food sciences, agriculture and horticulture. The Journal publishes papers describing significant novelty in the analysis of whole plants (including algae), plant cells, tissues and organs, plant-derived extracts and plant products (including those which have been partially or completely refined for use in the food, agrochemical, pharmaceutical and related industries). All forms of physical, chemical, biochemical, spectroscopic, radiometric, electrometric, chromatographic, metabolomic and chemometric investigations of plant products (monomeric species as well as polymeric molecules such as nucleic acids, proteins, lipids and carbohydrates) are included within the remit of the Journal. Papers dealing with novel methods relating to areas such as data handling/ data mining in plant sciences will also be welcomed.
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