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

作　　者：蔡霞 黄文静[1] 陈国权 CAI Xia;HUANG Wenjing;CHEN Guoquan(Guangdong Institute For Drug Control,Guangzhou,Guangdong 510163,China;Guangzhou Institute For Drug Control,Guangzhou,Guangdong 510160,China)

机构地区：[1]广东省药品检验所,广东广州510163 [2]广州市药品检验所,广东广州510160

出　　处：《今日药学》2019年第11期742-744,748,共4页Pharmacy Today

基　　金：广东省中医药局基金项目(20162033)

摘　　要：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 C18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,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 C18(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 to350.0 mg·kg^-1,the lowest quantification limits ranged from 274.0 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：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 

分 类 号：R917[医药卫生—药物分析学]