色谱

色谱 ›› 2018, Vol. 36 ›› Issue (9): 889-894.DOI: 10.3724/SP.J.1123.2018.04006

• 研究论文 • 上一篇    下一篇

固相萃取-超临界流体色谱-质谱联用同时快速测定中成药和保健食品中的12种抗过敏化学药物

杨直, 彭彦, 金朦娜, 林丽琴   

  1. 杭州市食品药品检验研究院, 浙江 杭州 310022
  • 收稿日期:2018-04-04 出版日期:2018-09-08 发布日期:2014-08-05
  • 通讯作者: 杨直,Tel:(0571)85463888,E-mail:manyangzhi@aliyun.com
  • 基金资助:

    浙江省食品药品监管系统科技计划项目（BH201601）.

Simultaneous rapid determination of 12 anti-allergic chemical drugs in Chinese traditional patent medicine and health food by supercritical fluid chromatography tandem mass spectrometry with solid phase extraction

YANG Zhi, PENG Yan, JIN Mengna, LIN Liqin   

  1. Hangzhou Institute for Food and Drug Control, Hangzhou 310022, China
  • Received:2018-04-04 Online:2018-09-08 Published:2014-08-05
  • Supported by:

    Science and Technology Project of Zhejiang Food and Drug Administration (No. BH201601).

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摘要：

建立了固相萃取-超临界流体色谱-质谱联用（SPE-SFC-MS/MS）快速检测中成药和保健食品中12种抗过敏化学药物的分析方法。样品经甲醇超声提取，Oasis MCX固相萃取柱净化。采用Waters Trefoil CEL1色谱柱（150 mm×3.0 mm，2.5 μ m），以CO2为流动相A，甲醇-氨水（100：0.1，v/v）为流动相B，进行梯度洗脱。流速为1.2 mL/min，柱温和背压分别为45℃和12.4×106 Pa。12种抗过敏化学药物以电喷雾离子源在正离子或负离子模式下用多反应监测（MRM）方式进行监测，整个分析过程在10 min内完成。结果表明，12种化学药物在5~250 μ g/L范围内线性关系良好，相关系数（r）均≥ 0.998，检出限（LOD）为0.141~0.262 μ g/L，定量限（LOQ）为0.703~1.308 μ g/L。3种加标水平（10、20和100 μ g/L）下，12种化学药物的平均回收率为76.1%~112.5%，相对标准偏差（RSD）为1.1%~8.3%。该法简便，灵敏性高，实用性强，可用于抗过敏类中成药和保健食品中非法添加抗过敏化学药物的检测。

关键词: 保健食品, 超临界流体色谱, 固相萃取, 抗过敏化学药物, 质谱, 中成药

Abstract:

An analytical method was developed for simultaneous rapid determination of 12 anti-allergic chemical drugs in Chinese traditional patent medicine and health food by supercritical fluid chromatography tandem mass spectrometry with solid phase extraction (SPE-SFC-MS/MS). Samples were extracted with methanol by sonification and then purified by Oasis mixed-model cation exchange SPE. The extracts were separated on a Waters Trefoil CEL1 (150 mm×3.0 mm, 2.5 μ m) column with a mobile phase consisting of carbon dioxide-methanol containing 0.1% (v/v) ammonia water in a gradient elution mode, at a flow rate of 1.2 mL/min. The column temperature was 45℃ and the back pressure was 12.4×106 Pa. The whole analysis was completed in 10 min. The 12 anti-allergic chemical drugs were detected by an electrospray ion source in positive or negative modes with a multiple reaction monitoring (MRM) mode. The calibration curves of the 12 anti-allergic chemical drugs showed good linearities in the range of 5-250 μ g/L with the correlation coefficients (r) ≥ 0.998. The limits of detection (LODs) were 0.141-0.262 μ g/L, and the limits of quantification (LOQs) were 0.703-1.308 μ g/L. The recoveries of the 12 anti-allergic chemical drugs at spiked levels of 10, 20 and 100 μ g/L were in the range of 76.1%-112.5%, and the relative standard deviations (RSDs) were 1.1%-8.3% (n=6). The method is simple, sensitive and reliable. It has been successfully used for the detection of illegally added anti-allergic chemical drugs in Chinese traditional patent medicine and health food.

Key words: anti-allergic chemical drug, Chinese traditional patent medicine, health food, mass spectrometry (MS), solid phase extraction (SPE), supercritical fluid chromatography (SFC)

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