超高效液相色谱-四极杆-飞行时间质谱法定性筛查保健食品中西地那非及其相关功效类非法添加化合物  

Qualitative analysis of illegally adulterated sildenafil and related compounds in dietary supplements by ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry

作　　者：于泓[1] 胡青[1] 孙健[1] 冯睿[1] 张甦[1] 张静娴[1] 毛秀红[1] 季申[1] YU Hong;HU Qing;SUN Jian;FENG Rui;ZHANG Su;ZHANG Jingxian;MAO Xiuhong;JI Shen(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《色谱》2018年第10期1005-1017,共13页Chinese Journal of Chromatography

基　　金：上海市科委技术平台专项(14DZ2294000);上海市科委"长三角科技联合公关领域"项目(18395810300);2017年国家食品药品监督管理总局食品补充检验方法项目~~

摘　　要：建立了超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF-MS)定性筛查102种西地那非及其相关功效化合物的方法。甲醇超声提取样品;采用Agilent Poroshell 120 SB-C18色谱柱(75 mm×3. 0 mm,2. 7μm),以0. 1%(v/v)甲酸水溶液-乙腈为流动相梯度洗脱,流速0. 4 mL/min;采用电喷雾离子(ESI)源,Q-TOF-MS作检测器,正离子模式检测;与对照品保留时间、母离子及碎片离子精确相对分子质量、元素组成比对,准确定性。西地那非等100种化合物在10种基质中的检出限为0. 1~50 mg/kg或0. 1~50 mg/L。并分类归纳了文中涉及的98种磷酸二酯酶5抑制剂质谱碎片裂解规律,为可疑物的识别和鉴定提供参考。该方法已应用于实际样品的测定,检出19种化合物,有效打击了非法添加行为。The presence of illegally adulterated sildenafil and related compounds in dietary supplements was qualitatively analyzed by employing ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry （UPLC-Q-TOF-MS）. Samples were extracted by ultrasonic method using methanol. The analysis was performed on an Agilent Poroshell 120 SB-C18 column （75 mm×3.0 mm, 2.7 μm） using gradient elution with a mixture of aqueous formic acid solution （0.1%, v/v） and acetonitrile as the mobile phase at a flow rate of 0.4 mL/min. Q-TOF-MS equipped with ESI ion source was operated in a positive ionization mode. Qualitative analysis was based on the retention time and the accurate relative molecular mass of elemental compositions of the precursor ion and product ions. The limits of detection （LODs） of sildenafil and other 99 compounds were found to be 0.1-50 mg/kg or 0.1-50 mg/L in 10 different matrices. In this manuscript, the fragmentation behavior of 98 phosphodiesterase-5 inhibitors are categorically summarized, which can provide information for referencing and identification of suspicious compounds. The method was successfully applied to the analysis of actual samples, of which 19 compounds combated the illegal adulteration behavior effectively.

关 键 词：超高效液相色谱-四极杆-飞行时间质谱 西地那非 磷酸二酯酶5抑制剂 保健食品 非法添加 

分 类 号：O658[理学—分析化学]