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海藻及其混伪品中17种氨基酸的含量测定 Δ

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张晓萍 ，张 文，戚鹏飞，朱仁愿，李 洁，张彩霞 ，邱国玉（兰州市食品药品检验所，兰州 730050）
中图分类号 R284.1 文献标志码 A 文章编号 1001-0408（2020）04-0468-05
DOI 10.6039/j.issn.1001-0408.2020.04.15

摘 要 目的：建立海藻及其混伪品中17种氨基酸的含量测定方法并进行聚类分析，为海藻药材的质量控制提供依据。方法：取
18批样品（S1～S6为真品、S7～S18为混伪品），经酸水解后，采用氨基酸全自动分析仪测定氨基酸含量。色谱柱为LCAK06/Na型
磺酸基强酸性阳离子交换树脂分离柱，流动相为缓冲液-再生液系统（梯度洗脱），流速为洗脱泵0.45 mL/min、衍生泵0.25 mL/min，
检测波长为440 nm（脯氨酸）、570 nm（其余氨基酸），进样量为50 μL。采用PASW Statistics 18.0软件，以“平方Euclidean距离”为
度量标准使用组间联接的聚类方法对 18批样品进行聚类分析。结果：17种氨基酸均分离良好，空白无干扰；其质量浓度与峰面积
的线性关系良好（r均大于0.998），线性范围上下限分别为48.06 μg/L（胱氨酸）、1.501 μg/L（甘氨酸）；精密度、重复性、稳定性试验
RSD均小于2％；平均加样回收率为90.60％～101.56％（RSD为0.88％～2.15％，n＝6）。海藻及其混伪品样品中均检出17种氨基
酸，其中谷氨酸、天冬氨酸、亮氨酸、丙氨酸、甘氨酸、缬氨酸的含量相对较高。聚类分析结果显示，18批样品可以聚为4类，S1～S6
为一类，S7～S9为一类，S10～S12 、S16～S18为一类，S13～S15为一类，与海藻真品与其混伪品的鉴定结果相一致。结论：该方法
操作简便、快速、准确度高、重复性好，可用于海藻及其混伪品的氨基酸定量分析及真伪区分。
关键词 海藻；混伪品；阳离子交换色谱法；柱后衍生；氨基酸

Content Determination of 17 Kinds of Amino Acids in Sargassum and Its Adulterants
ZHANG Xiaoping，ZHANG Wen，QI Pengfei，ZHU Renyuan，LI Jie，ZHANG Caixia，QIU Guoyu（Lanzhou
Institute for Food and Drug Control，Lanzhou 730050，China）

ABSTRACT OBJECTIVE：To establish the method for content determination of 17 kinds of amino acids in Sargassum and its
adulterants，and to carry out cluster analysis，so as to provide reference for quality control of Sargassum. METHODS：Totally of
18 batches of sample （S1-S6 as certified product，S7-S18 as adulterants） were collected. After acid hydrolysis，amino acids
contents were detected by using automatic amino acid analyzer. The separation was performed on LCAK06/Na sulfonic acid cation
exchange resin column with mobile phase consisted of buffer-regeneration system（gradient elution）at the flow rate of 0.45 mL/min
（elution pump）and 0.25 mL/min（derivative pump）. The detection wavelengths were set at 440 nm（proline）and 570 nm（other
amino acids），and the sample size volume was 50 μL. PASW Statistics 18.0 software was used，and cluster analysis was conducted
by using group connection method of cluster analysis with“square Euclidean distance”as the measurement standard. RESULTS：17
kinds of amino acids were well separated without interference from blank sample. The linear relationship between mass
concentration and peak area was good（all r were over 0.998），and the upper and lower limits of the linear range were 48.06 μg/L
（cystine）and 1.501 μg/L（glycine），respectively；RSDs of precision，reproducibility and stability tests were lower than 2％. The
average recoveries were between 90.60％-101.56％（RSDs were 0.88％-2.15％，n＝6）. 17 kinds of amino acids were detected in
Sargassum and its adulterants，among which the contents of glutamic acid，aspartic acid，leucine，alanine，glycine and valine were
relatively high. Results of cluster analysis showed that 18 batches of sample were clustered into 4 categories，i.e. S1-S6 into one
category；S7-S9 into one category；S10-S12，S16-S18 into one category；S13-S15 into one category；which was consistent with
the identification result of Sargassum and its adulterants. CONCLUSIONS： The method is simple， rapid， accurate and
reproducible，and can be used for the quantitative analysis and identification of amino acids in Sargassum and adulterants.
KEYWORDS Sargassum；Adulterants；Cation exchange chromatography；Post-column derivatization；Amino acids

海藻为海产藻类植物的总称。中药海藻（以下简称 为马尾藻科植物海蒿子[Sargassum pallidum（Turn.）C.
“海藻”）始载于《神农本草经》，列为中品，具有软坚散 Ag.]或羊栖菜[S. fusiforme（Harv.）Setch.]的干燥藻体，前
[2]
结、消痰、利水之功效，多用于瘿瘤、瘰疬、睾丸肿痛、痰 者习称“大叶海藻”，后者习称“小叶海藻”。但是目前
[1]
饮水肿等症 。2015年版《中国药典》（一部）收载的海藻 市 场 上 除 药 典 收 载 的 品 种 外 ，尚 有 铜 藻 [S. horneri
（Turn.）C. Ag.]、亨氏马尾藻[S. henslowianum C. Ag.]、瓦
Δ 基金项目：甘肃省食品药品科研项目（No.2018GSFDA020）
氏马尾藻[S. vachellianum Grev.]和海黍子[S. kjellmania-
＊主管中药师，硕士。研究方向：药物分析、中药质量控制。电
num Yendo.]等其他藻类植物冒充海藻大量流通，不仅干
话：0931-2312648。E-mail：187253373@qq.com
扰了药材市场的正常运行，还会影响用药的安全有效
# 通信作者：副主任中药师。研究方向：中药材质量评价及资源
开发利用。电话：0931-2312648。E-mail：917927942@qq.com 性 [3-6] 。

·468 · China Pharmacy 2020 Vol. 31 No. 4 中国药房 2020年第31卷第4期