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高通量高效液相色谱法快速检测西红花中15种非法添加色素

花匠小妙招
2025-09-09 19:39

化学分析计量CHEMICAL ANALYSIS AND METERAGE 第30卷，第1期

2021年1月V ol. 30，No. 1Jan. 202129doi ：10.3969／j.issn.1008–6145.2021.01.006

高通量高效液相色谱法快速检测西红花中

15种非法添加色素

曹雅静，刘丛丛，赖宇红

(广东省药品检验所，广州　510663)

摘要　建立高通量的高效液相色谱法同时检测15种西红花中非法添加色素，对于阳性样品采用液相色谱–质

谱联用法确证。采用Poroshell 120 EC–C 18色谱柱(100 mm ×4.6 mm ，

2.7 μm)分离，以甲醇–0.02 mol ／L 乙酸铵溶液（用氨水调pH 至5.9±0.05）进行梯度洗脱，流量为1.2 mL ／min ，柱温为35 ℃，以450 nm 和500 nm 双波长检测。缓冲盐pH 值和流动相流量对色谱条件影响大，需严格控制。该方法重现性好，各物质分离度均大于1.5，标准曲线

的线性相关系数r 为0.998～1.000，

样品高、中、低浓度的加标回收率为70.1%～93.1%，测定结果的相对标准偏差为1.2%～6.6%(n =6)，检出限为0.01～0.05 mg ／kg 。该方法精密度良好，分析时间短，分析结果稳定，可用于中药材西红花中15种非法添加色素的快速筛查和含量测定，同时能为相关部门制定监督抽检中药材染色掺伪的补充检验方法。

关键词　非法染色；西红花；高通量；高效液相色谱法；液相色谱–质谱联用法

中图分类号：O657.7 文献标识码：A 文章编号：1008–6145(2021)01–0029–06

Rapid detection of 15 illegal additive pigments in Crocus Sativus by high throughput HPLC

Cao Yajing ， Liu Congcong ， Lai Yuhong

(Guangdong Institute for Drug Control ， Guangzhou 　510663， China)

Abstract 　A high throughput high performance liquid chromatography(HPLC) was established for the simultaneous determination of 15 pigments added illegally in Crocus Sativus and the positive samples were confirmed by liquid chromatography mass spectrometry (LC–MS). The chromatographic column Poroshell 120 EC–C 18 (100 mm ×4.6 mm ，

2.7 μm) was used as separation column ，gradient elution was conducted using methanol–0.02 mol ／L ammonium acetate solution (adjusted to a pH of 5.9±0.05). The column temperature was 35 ℃，and the flow rate was 1.2 mL ／min ，the detection wavelength was 450 nm and 500 nm. The chromatographic conditions were affected by the pH value and flow rate of buffer salts which should be controlled strictly. The method has good reproducibility ，the separation degree of each substance was more than 1.5. The linear correlation coefficient (r ) of the standard curve was 0.998–1.000，the standard recoveries of high ，medium and low concentration addition were 70.1%–9

3.1% with the RSD of 1.2%–6.6%(n =6)，the detection limit was 0.01–0.05 mg ／kg. The method can be used for rapid screening and content determination of 15 pigments added illegally in Crocus Sativus with the good precision ，short analysis time ，stable analysis result ，and it can also be used for the establishment of a supplementary inspection method to supervise and spot-check the adulteration and dyeing of crocus sativus.

Keywords 　illegal dyeing; Crocus Sativus; high throughput; HPLC; LC–MS ／MS

西红花是一种名贵的中药材，为鸢尾科植物番

红花(Crocus Sativus L.)的干燥柱头［1］。根据《中国

药典》2015年版记载，该药材具有活血化瘀、凉血解毒、解郁安神的功效。西红花可用于经闭症癥瘕、产

基金项目　广东省中医药局项目（20191042）通讯作者　刘丛丛，主管药师，硕士研究生，从事中药材中非法添加成分的检测，*****************

收稿日期　2020–10–26

引用格式　曹雅静，刘丛丛，赖宇红.高通量高效液相色谱法快速检测西红花中15种非法添加色素［J ］.化学分析计量，2021，30(1): 29.

Cao Yajing ，Liu Congcong ，Lai Yuhong. Rapid detection of 15 illegal additive pigments in Crocus Sativus by high throughput HPLC ［J ］. Chemical Analysis and Meterage ，2021，30(1): 29.