今日药学

2019, v.29(11) 742-744+748

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降压类健康产品中3种非法添加化学成分的检测及确证方法研究
Determination and Conformation of 3 Chemicals Illegally Added in Antihypertensive Healthy Products

蔡霞;黄文静;陈国权;
CAI Xia;HUANG Wenjing;CHEN Guoquan;Guangdong Institute For Drug Control;Guangzhou Institute For Drug Control;

摘要(Abstract):

目的建立降压类健康产品中3种非法添加化学成分的高效液相色谱检测法及液相色谱-质谱联用确证方法。方法采用ACE C_(18)色谱柱(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.2%磷酸溶液为流动相,梯度洗脱,检测波长为220 nm,外标法定量,液质联用法进一步定性确证。结果 3种成分在5.0~100.0 mg·L(-1)范围内线性关系良好,方法检出限为83.0~350.0 mg·kg(-1)范围内线性关系良好,方法检出限为83.0~350.0 mg·kg(-1),定量下限为274.0~1 155.0 mg·kg(-1),定量下限为274.0~1 155.0 mg·kg(-1),平均加样回收率在99.4%~102.0%之间,RSD在1.3%~1.9%之间。结论该方法准确可靠、简便快捷,适用于降压类健康产品中非法添加化学物质的检测。
OBJECTIVE To established a method for the determination and conformation of 3 chemicals illegally added in antihypertensive healthy products. METHODS The chromatographic separation was achieved on an ACE C_(18)(250 mm× 4. 6 mm,5 μm) column with the mobile phase of acetonitrile-0. 2% phosphoric acid solution by gradient elution,at the detection wavelength of 220 nm,quantification analysis were performed by the extent standard method. The positive samples were further identified and verified by LC-MS/MS. RESULTS It was linear in the range of 5. 0-100. 0 mg·L(-1),平均加样回收率在99.4%~102.0%之间,RSD在1.3%~1.9%之间。结论该方法准确可靠、简便快捷,适用于降压类健康产品中非法添加化学物质的检测。
OBJECTIVE To established a method for the determination and conformation of 3 chemicals illegally added in antihypertensive healthy products. METHODS The chromatographic separation was achieved on an ACE C_(18)(250 mm× 4. 6 mm,5 μm) column with the mobile phase of acetonitrile-0. 2% phosphoric acid solution by gradient elution,at the detection wavelength of 220 nm,quantification analysis were performed by the extent standard method. The positive samples were further identified and verified by LC-MS/MS. RESULTS It was linear in the range of 5. 0-100. 0 mg·L(-1). The detection limits ranged from 83. 0 mg·kg(-1). The detection limits ranged from 83. 0 mg·kg(-1) to350.0 mg·kg(-1) to350.0 mg·kg(-1),the lowest quantification limits ranged from 274.0 mg·kg(-1),the lowest quantification limits ranged from 274.0 mg·kg(-1) to 1 155.0 mg·kg(-1) to 1 155.0 mg·kg(-1),the average recoveries were in the range of 99.4%-102.0% and RSD were in the range of 1. 3%-1. 9%. CONCLUSION The method is accurate and reliable,simple and rapid,suitable for the determination of chemicals illegally added in antihypertensive healthy products.

关键词(KeyWords): 降压类健康产品;非法添加;高效液相色谱法;液相色谱-质谱联用法
healthy products for antihypertension;illegal additives;HPLC;LC-MS/MS

Abstract:

Keywords:

基金项目(Foundation): 广东省中医药局基金项目(20162033)

作者(Authors): 蔡霞;黄文静;陈国权;
CAI Xia;HUANG Wenjing;CHEN Guoquan;Guangdong Institute For Drug Control;Guangzhou Institute For Drug Control;

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