液相色谱串联质谱同时测定不同基质保健食品中20种利尿剂  

Simultaneous determination of 20 diuretics in dietary supplements with different matrixes by liquid chromatography tandem mass spectrometry

作　　者：张建丽[1] 王占良[1] 张亦农[1] 

机构地区：[1]国家体育总局反兴奋剂中心,北京100029

出　　处：《分析试验室》2015年第7期840-846,共7页Chinese Journal of Analysis Laboratory

摘　　要：采用液相色谱串联质谱技术,分别建立了固体基质和液体基质保健食品中20种利尿剂的测定方法。两种不同基质的保健食品分别经过相应的化学前处理后,经Agilent Zorbax SB-C183.5μm×100 mm×2.1 mm色谱柱分离分析,以10 mmol/L甲酸铵（pH 3.5）和乙腈为流动相进行梯度洗脱,电喷雾正负离子切换多反应监测模式采集。20种利尿剂在线性范围内线性关系良好,R2大于0.99。固体基质中低、中、高3个浓度的回收率为59.5%~115.9%,RSD≤7.8%;液体基质中低、中、高3个浓度的回收率为57.4%~121.1%,RSD≤8.1%。方法适用于保健食品非法添加的常规检测。Diuretics can be illegally added into dietary supplements which have the functions of weight losing or blood pressure reduction. Diuretics as a kind of stimulants have been prohibited by world anti-doping agency （WADA）. In order to protect athletes to avoid taking these dietary supplements accidentally, a liquid chromatography tandem mass spectrometry （LC-MS/MS） method for separation and determination of 20 diuretics in dietary supplements is developed. Preparation methods for two kinds of different matrixes including solid matrix and liquid matrix have been studied with liquid liquid extractions followed by validations. The mobile phase consisted of 0.01 mol/L ammonium formate buffer （pH 3.5 ） and acetonitrile by gradient elution. Compounds were analyzed using positive and negative electrospray ionization scanning at the same time by multi- reaction monitoring （MRM） mode in a triple quadrupole spectrometryl The extraction recoveries were from 59.5% to 115.9% in solid matrix and from 57.4% to 121.1% in liquid matrix. Good linearities were obtained in their linearity ranges both in solid matrix and liquid matrix. The precisions were no more than 7.8% in solid matrix and no more than 8.1% in liquid matrix. This method was firstly reported for simultaneous determination of 20 diuretics in dietary supplements with different matrixes and suitable for routine analysis.

关 键 词：利尿剂 保健食品 液相色谱串联质谱 

分 类 号：TS207.3[轻工技术与工程—食品科学]