论文总字数：23338字

摘 要

苯二氮䓬类（Benzodiazepines, BZDs）物质是一种精神类药物，在临床上有合理的应用范围，但此类药物被不法商家非法利用于保健品中。目的：本论文选取十种非法添加物质作为研究对象，建立了一种高效液相色谱法对选定物质进行测定，实现对安神类保健品中非法添加物的快速测定。方法：使用三氯甲烷超声提取，以甲醇-乙腈-甲酸（pH=3.4）为流动相，梯度分离。分离结果用紫外光检测，检测波长为230nm，进行高效液相色谱法测定。结果：相关组分有很好的分离效果，检测在40分钟内完成，响应峰形良好，各组分清晰可见。十种物质矫正曲线的R²值分别为0.99948、0.99975、0.99943、0.99953、0.99935、0.99951、0.99951、0.99956、0.99923、0.99919，皆高于0.999，说明校正曲线在0~25μg/L范围内具有良好的线性关系。各组分的RSD值均低于5%，测量结果接近真实值，且大部分物质回收率在90%~110%范围内。在此条件下十种物质的检出限分别为0.3129、0.0600、0.2177、0.2150、0.1172、0.0782、0.1039、0.1746、0.1024、0.0699。结论：该方法可行有效，提高了检测效率，可作为安神类保健品中十种精神类药物的合理检测方法。

关键词：苯二氮䓬类 高效液相色谱法 保健食品

Study on Simultaneous Determination of ten illegal drugs, Benzodiazepines, in health products by High Performance Liquid Chromatography

Abstract

Benzodiazepines (BZDs) are a kind of psychotropic drugs, which have been reasonably applied to clinical medicine. But these drugs are illegally used in health care products by some producers without social responsibility. Purpose. The purpose of this work was to build a method which allowed 10 kinds of benzodiazepines to be simultaneously detected by using high performance liquid chromatography (HPLC), to separate and detect illegal additives in the health care products. Method. Extract BZDs from samples by using trichloromethane as the extraction liquid. A gradient of methanol-acetonitrile-formic acid (pH = 3.4) was used as the mobile phase for separation. The samples were detected using a UV detector, and the detection wavelength was 280nm. Results. The relevant components had a good separation result- all of the response peaks had good and clear shape, and the detection completed in 40 minutes. The R² values of 10 correction curves are 0.99948, 0.99975, 0.99943, 0.99953, 0.99935, 0.99951, 0.99951, 0.99956, 0.99923 and 0.99919, which were higher than 0.999, indicating that the calibration curve had a good linear in the range of 0~25μg/L. The relative standard deviation was less than 5%, indicating that the measurement results close to the true value. And the percentage of most of recoveries was between 90% and 110%. Under the condition, the detection limits were 0.3129, 0.0600, 0.2177, 0.2150, 0.1172, 0.0782, 0.1039, 0.1746, 0.1024 and 0.0699. Conclusion. The method is feasible and effective, and improves the detection efficiency. It can be used as a reasonable method to detect 10 kinds of psychotropic drugs in the health care products.

Keywords: BZDs; HPLC; health products

目 录

摘要 I

Abstract II

第一章 引言 1

1.1 保健食品 1

1.1.1 安神类保健产品发展现状 1

1.2 苯二氮䓬类药物介绍 1

1.2.1 BZDs理化特性 2

1.2.2 使用现状 2

1.3 检测方法 2

1.3.1 薄层色谱法 2

1.3.2 气相色谱法 3

1.3.3 高效液相色谱法 3

1.3.4. 液相色谱-串联质谱(LC-MS/MS)法 4

1.3.5 胶体金法（试剂盒） 4

1.4 选题的目的及意义 4

第二章 方法学评价 6

2.1 实验材料 6

2.1.1 样品 6

2.1.2 标准品及试剂 6

2.1.3 主要仪器设备 7

2.2 标准曲线 7

2.2.1 混合标准储备液的制备 7

2.2.2 标准曲线的制备 8

2.3 样品前处理 8

2.4 色谱优化 8

2.4.1 色谱条件 8

2.4.2 流动相 8

2.4.3 检测器 9

2.4.4 柱温箱温度 9

2.4.5 进样量 9

2.5 回收率的测定 9

2.6 精密度的测定 9

2.7 检出限与定量限 10

第三章 实验结果与分析 11

3.1 实验结果与分析 11

3.1.1 检测波长的选定 11

3.1.2 流动相比例的选定 17

3.1.3 各物质校正曲线 19

3.1.4 准确度的测定结果 24

3.1.5 精密度的测定结果 35

3.1.6 检出限和定量限的计算结果 36

3.2 样品检测结果 37

第四章 结论与展望 38

4.1 结论 38

4.2 展望 38

参考文献 39

致谢 41

第一章 引言

1.1 保健食品

保健食品具有特定保健功能，适宜于特定人群食用。如今处于亚健康的人群数量不断上升，亚健康的问题也得到更多人的重视，在《中国城市健康白皮书》中显示，主要城市的白领人群中，真正的“健康人”只有2.5%^[1]。大部分城市人群处于亚健康状态，多患有代谢紊乱疾病，且容易疲劳并受失眠困扰，部分人患有不同程度的心理疾病。在这种情况下，加之现如今消费水平的上升，人们对保健食品的接受程度逐年增加。

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