目的 建立超高效液相色譜熒光（UHPLC-FLD）法同時測定大黃中大黃素、蘆薈大黃素、大黃酸、大黃酚、大黃素甲醚和大黃素-8-O-β-D-葡萄糖苷的含量，并應用于10個不同產地大黃飲片的分析。方法 大黃粉末經(jīng)甲醇提取制備供試品溶液，采用Agilent Poroshell 120 EC-C₁₈柱（50 mm×4.6 mm，2.7 μm）；流動相為0.1%甲酸水溶液（A）-0.1%甲酸甲醇（B），梯度洗脫；體積流量0.6 mL·min^-1；柱溫30℃；熒光檢測器激發(fā)波長435 nm，發(fā)射波長515 nm。進行專屬性、線性關系、定量限及檢出限、精密度、穩(wěn)定性、重復性、加樣回收率考察。應用已建立的方法分析10個不同產地大黃飲片中6種大黃蒽醌含量。結果 6種成分在各自范圍內線性關系良好，精密度、穩(wěn)定性、重復性均良好；平均加樣回收率為97.86%～103.2%，RSD為1.27%～2.15%。10個不同產地大黃飲片中蒽醌總量均符合《中國藥典》要求；但不同產地的大黃中蒽醌單體的含量差別較大。結論 建立的UHPLC-FLD法靈敏、快速、準確、穩(wěn)定且重復性好，可用于大黃中6種大黃蒽醌的含量測定。

Objective To establish a UHPLC-FLD method for the simultaneous determination of emodin, aloe emodin, rhein, chrysophanic acid, emodin-3-methyl ether and emodin-8-O-β-D-glucoside in Rhei Radix et Rhizom decoction pieces. Methods The analysis of methanol extract of Rhei Radix et Rhizom decoction piece was performed on a 30 ℃ thermostatic Agilent Poroshell 120 EC-C ₁₈ column (50 mm×4.6 mm, 2.7 μm), with the mobile phase comprising of 0.1% formic acid water (A) -0.1% formic acid methanol (B) flowing at 0.6 mL·min^-1 in a gradient elution manner, and the excitation wavelength and emission wavelength were set at 435 nm and 515 nm, respectively. Specificity, linear relationship, limit of quantitation and detection, precision, stability, repeatability and recovery were investigated. The established method was used to analyze the anthraquinone content of six kinds of rhubarb from 10 different areas. The established method was used to analyze the anthraquinone content of six kinds of rhubarb from 10 different areas. Results Six constituents showed good linear relationships within their own ranges. Precision, stability and repeatability all meet the testing requirements. whose average recoveries were 97.86% — 103.2% with the RSDs of 1.27% — 2.15%. The total amount of anthraquinone in 10 Rhei Radix et Rhizoma decoction pieces from different origins met the requirements of pharmacopoeia. However, the content of anthraquinone monomer in Rhei Radix et Rhizoma decoction pieces from different producing areas varies greatly. Conclusion The method is sensitive, rapid, accurate, stable and reproducible, and can be used for the determination of related compounds in Rhei Radix et Rhizom.

R284.1

北京市自然科學基金(7214284);中央高校基本科研業(yè)務費專項資金(2020-JYB-ZDGG-105);國家自然科學基金(81573839)