【摘要】：建立了固相萃取(SPE)-定量核磁共振波譜(qNMR)技術(shù)測定板藍(lán)根飲片中有效成分表告依春含量的方法。樣品用水超聲提取兩次,采用SPE對提取液進(jìn)行富集濃縮,用q NMR測定表告依春的含量。考察了樣品預(yù)處理和qNMR實(shí)驗(yàn)條件對測定結(jié)果的影響,選擇氘代二甲基亞砜為溶劑,用基準(zhǔn)試劑鄰苯二甲酸氫鉀標(biāo)定的2,3,5-三碘苯甲酸為內(nèi)標(biāo),選擇脈沖寬度P_1=14.1μs,延遲時(shí)間d_1=5 s,掃描次數(shù)N_S=256為qNMR定量測定表告依春的最佳實(shí)驗(yàn)條件。表告依春的定量峰為δ5.365~5.399(H-7b,d,1H)。結(jié)果表明,日內(nèi)測量精密度(RSD)為0.5%,日間精密度為0.8%,表告依春與三碘苯甲酸峰面積比與質(zhì)量比的零截距標(biāo)準(zhǔn)曲線線性相關(guān)系數(shù)為0.9991,且斜率與理論值相符。根據(jù)響應(yīng)值標(biāo)準(zhǔn)偏差和標(biāo)準(zhǔn)曲線斜率法確定此法測定表告依春的檢測限(LOD)為0.05 mg/g;定量限(LOQ,S/N≥150)為0.19 mg/g。包括樣品提取過程的表告依春的回收率為97.4%~101.7%。采用本方法測定板藍(lán)根飲片中的表告依春的含量為0.19~1.26 mg/g。研究結(jié)果表明,采用SPE進(jìn)行富集,擴(kuò)大了q NMR的應(yīng)用范圍,可用于低含量復(fù)雜樣品的定量分析。
[Abstract]:A solid-phase extraction (SPE)-quantitative nuclear magnetic resonance spectroscopy (qNMR) technique was established to determine the content of indigowoad root in Radix Isatidis decoction pieces. The sample was extracted twice with water, and the extract was concentrated by SPE, and the content of Eichun was determined by q-NMR. The effect of sample pretreatment and qNMR experiment conditions on the determination results was studied. The determination of the effect of the sample pretreatment and qNMR experiment conditions on the determination results was studied. The 2,3,5-triiodobenzoic acid was used as the internal standard, and the pulse width, P _ 1 = 14.1. m, and the delay time d _ 1 = 5 s, were chosen as the internal standard. The number of scans N _ S = 256 is the best experimental condition for qNMR quantitative determination of Eichun. The quantitative peak of Eichun was 5.365-5.399 (H-7b, d, 1H). The results showed that the RSD was 0.5% and the day-day precision was 0.8%. The linear correlation coefficient of the peak area ratio of Eichun to triiodobenzoic acid and the mass ratio was 0.9991, and the slope was in line with the theoretical value. The detection limit (LOD) for the determination of Eichun according to the standard deviation of the response and the slope of the standard curve was 0.05 mg/ g; the limit of quantitation (LOQ, S/ N-150) was 0.19 mg/ g. And the recovery rate of the epideochun, which comprises the sample extraction process, is 97.4% to 101.7%. The content of the epidesulin in the radix isatidis decoction pieces is determined to be 0.19 to 1.26 mg/ g by the method. The results show that the application range of q-NMR is expanded by SPE, and can be used for quantitative analysis of complex samples with low content.
【作者單位】： 上海應(yīng)用技術(shù)大學(xué)化學(xué)與環(huán)境工程學(xué)院;
【基金】：國家自然科學(xué)基金項(xiàng)目(No.31671928) 上海市自然科學(xué)基金項(xiàng)目(No.15ZR1440800)資助~~
【分類號】：O657;R286.0

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