目的 建立板藍(lán)根顆粒及組分中糖類成分的快速定性方法和主要單糖的定量測(cè)定方法。方法 采用超高效液相色譜結(jié)合質(zhì)譜檢測(cè)器（UPLC-MS）快速定性板藍(lán)根顆粒及組分中的糖類成分，采用超高效液相色譜結(jié)合蒸發(fā)光散射檢測(cè)器（UPLC-ELSD）同時(shí)測(cè)定果糖、葡萄糖的含量。使用ACQUITY UPLC BEH Amide（2.1 mm×150 mm，1.7 μm）色譜柱分離，柱溫35℃。流動(dòng)相分別為乙腈-0.1%氨水（含10 mmol/L碳酸氫銨）（75：25）和乙腈（含0.2%三乙胺）-水（75： 25），體積流量0.2 mL/min。質(zhì)譜檢測(cè)器采用負(fù)離子模式，毛細(xì)管電壓0.8 V，錐孔電壓4 V，探頭溫度600℃，采集頻率1 Hz，采用全掃描及SIR掃描模式。ELSD檢測(cè)器漂移管溫度50℃，氮?dú)鈮毫?75.8 kPa。結(jié)果 經(jīng)UPLC-MS法鑒定板藍(lán)根顆粒中糖類成分種類為單糖和雙糖，主要為果糖、葡萄糖、蔗糖、肌醇，水洗脫組分檢出果糖、葡萄糖、蔗糖，10%醇洗脫組分和20%醇洗脫組分均檢出蔗糖。UPLC-ELSD法含量測(cè)定結(jié)果表明，果糖、葡萄糖在各自范圍內(nèi)線性關(guān)系良好，各相關(guān)系數(shù)均0.999 3在以上，平均回收率分別為99.0%、100.1%。28個(gè)生產(chǎn)企業(yè)的28批樣品糖類成分含量差異較大。結(jié)論 所建立的方法準(zhǔn)確度、重復(fù)性良好，具有操作簡(jiǎn)便、節(jié)省時(shí)間等特點(diǎn)，可為板藍(lán)根顆粒的質(zhì)量控制和物質(zhì)基礎(chǔ)研究提供參考。

Objective A rapid qualitative method for the Sugars and a quantitation method for the main monosaccharides in Banlangen Granule and its fractions were established. Methods Sugars were determined by ultra performance liquid chromatography (UPLC) method combined with mass spectrometric detector (MS). Fructose and glucose were determined by UPLC method combined with evaporative light scattering detector (ELSD). Separation was performed on an ACQUITY UPLC BEH Amide (2.1 mm×150 mm,1.7 μm) column and the column temperature was 35℃. The mobile phase consisted of acetonitrile (containing 0.2% triethylamine)-water (75:25) and acetonitrile-water (containing 0.1% ammonia and 10 mmol/L NH₄HCO₃) (75:25) at a flow rate of 0.2 mL/min. The MS spectra were acquired in negative mode with a capillary voltage of 0.8 kV, a cone voltage of 4.0 kV, a probe temperature of 600℃, an acquisition frequency of 1 Hz. The analytes were determined in full scan mode and SIR mode. The temperature for the evaporator tube of ELSD was maintained at 50℃ and the gas pressure for nitrogen was 275.8 kPa. Results The types of Sugars in Banlangen Granule were monosaccharide and disaccharide. Fructose, glucose, sucrose and inositol in the sample of banlangen granules were detected by UPLC-MS method. Fructose, glucose and sucrose were detected in water fraction. Sucrose was detected in both 10% alcohol fraction and 20% alcohol fraction. The results of UPLC-ELSD method showed that the calibration curves of the 2 components showed good linearity within their test ranges. The correlation coefficients were not lower than 0.9993. The average recoveries for fructose, glucose were 99.0%, 100.1%, respectively. There was a great variation among contents of sugars in 28 batches of samples from 28 manufactures. Conclusion The proposed method was accurate, repeatable, simple and fast, thus providing reference for quality control and basic substances research of Banlangen Granule.

R286.02

國(guó)家自然科學(xué)基金（81303194）；重大新藥創(chuàng)制專項(xiàng)課題（2018ZX09735006）；中國(guó)食品藥品檢定研究院學(xué)科帶頭人培養(yǎng)基金（2017X1）