李名洁，王 玉，陈 搏，孙代华，王泽霞，陈志元

（劲牌持正堂药业有限公司，湖北省中药配方颗粒工程技术研究中心，湖北黄石 435100）

摘要：建立固相萃取-高效液相色谱法测定不同地域及季节桑叶中1-脱氧野尻霉素（DNJ）含量，了解不同地域桑叶DNJ含量变化规律从而确定最佳的桑叶采摘区域和采摘期。采用固相萃取对桑叶药材提取液中的DNJ净化、富集，用高效液相色谱测定含量。色谱柱为Shodex Asahipak NH50（4.6 m×250 mm，5 μm），蒸发光散射检测器，漂移管温度为100 ℃，流动相为乙腈-6.5 mmol/L乙酸铵水溶液（82∶18，V/V）等度洗脱，流动相流速为1.0 mL/min，进样量为 10 μL。DNJ 在 84.39-421.9 mg/L 范围内线性关系良好（相关系数 R²＝0.999 7），平均回收率为 100.6%，RSD 为1.27%。桑叶中DNJ在不同季节和不同地域间存在显著性差异。该方法简便、准确、重现性好，可用于桑叶中DNJ含量的测定。

关键词：固相萃取；桑叶；1-脱氧野尻霉素；强酸性阳离子交换树脂

中图分类号：TS207.3   文献标识码：A   文章编号：1674-506X（2020）05-0123-0005

Content of 1-deoxynojirimycin in Mulberry Leaf from Different Regions and Different Harvest Time

LI Ming-jie, WANG Yu, CHEN Bo, SUN Dai-hua, WANG Ze-xia, CHEN Zhi-yuan

（Jing Brand Chizhengtang Pharmaceutical Co., Ltd., Hubei TCM Formula Granule Engineering & Technology Research Center, Huangshi Hubei 435100, China）

Abstract：To establish a solid-phase extraction with high-performance liquid chrom-atography method for the determination of 1-deoxynojirimycin (DNJ) in mulberry leaf and contrast the content of DNJ in different seasons. Exploring the natural change rule of DNJ content along with the change of seasons and regions, to determine the best harvesting period and harvesting region. Using solid-phase extraction to purified and enriched the DNJ of mulberry leaf extract solution. The HPLC method was established using Shodex Asahipak NH50 column (4.6 m×250 mm, 5 μm) with acetonitrile-water (V/V＝82∶18, containing 6.5 mmol/L ammonium acetate) as mobile phase. Flow rate was 1 mL/min, and injection volume was 10 μL. The samples were tested on evaporative light scattering detector with drift tube temperature of 100 ℃. The calibration curve was linear over the concentration range from 84.39 mg/L to 421.9mg/L (R²＝0.999 7), the average recovery was 100.6% (RSD＝1.27%). The results showed that the content of DNJ was significantly different in different seasons and regions. This method was simple, rapid, and accurate and was suitable for the determination of DNJ in mulberry leaf.

Keywords：solid-phase extraction; mulberry leaf; 1-deoxynojirimycin; strong-acid cation exchange resin

doi：10.3969/j.issn.1674-506X.2020.05-023

收稿日期：2020-04-13

基金项目：国家重点研发计划（2017YFC1702400）

作者简介：李名洁（1991-），硕士，工程师。研究方向：中药现代化。

引文格式：李名洁,王玉,陈搏,等.不同产地及季节桑叶中DNJ的含量测定[J].食品与发酵科技,2020,56(5):123-127.