液相色谱-串联质谱法测定枸杞酒中11种PDE-5抑制剂和4种α-受体阻断剂  

Rapid determination of 11 PDE-5 inhibitors and 4α-receptor blockers in wolfberry wine by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：韩瑨烜 李婷娜 阿力木·阿布都 马媛 HAN Jinxuan;LI Tingna;ALIMU·Abudu;MA Yuan(Xinjiang Uygur Autonomous Region product quality supervision and Inspection Institute,Urumqi 830011,China)

机构地区：[1]新疆维吾尔自治区产品质量监督检验研究院,乌鲁木齐830011

出　　处：《化学分析计量》2023年第4期15-19,共5页Chemical Analysis And Meterage

基　　金：新疆维吾尔自治区自然科学基金(2020D01A81);2020年度自治区市场监督管理局科技计划项目(202003)。

摘　　要：建立了基于超高效液相色谱-串联质谱法对枸杞酒中11种PDE-5抑制剂和4种α-受体阻断剂的快速筛查方法。样本经1%甲酸-甲醇提取,超声波水浴20 min助提,以Hypersil GOLD C18为分离柱,0.1%甲酸-水/甲醇为流动相,梯度洗脱,以超高效液相色谱-质谱联用仪在多反应监测模式(MRM)下分析。采用该方法,15种违禁药物可以在10 min分析完毕,各组分离子色谱图峰形良好,保留时间在2.21~7.76 min之间。各组分质量浓度在5~100μg/L线性范围内相关系数均大于0.99,检出限为32.5~60.6μg/kg,定量限为97.5~157.5μg/kg,在80、40、20μg/kg三个加标水平下15种违禁药物回收率为78.8%~118.8%,相对标准偏差均小于10%(n=6)。该方法具有操作简便、分析快速、基质干扰小等优点,适用于枸杞酒中多种壮阳类违禁药物的筛查。A rapid screening method for 11 PDE-5 inhibitors and 4α-receptor blockers in wolfberry wine was established based on ultra-high performance liquid chromatography-tandem mass spectrometry.The samples were extracted with 1%formic acid-methanol,assisted by ultrasonic water bath for 20 min,with Hypersil GOLD C 18 as separation column,0.1%formic acid-water/methanol as mobile phase,gradient elution procedure,by ultra-high performance liquid chromatography-mass spectrometry in multiple reaction monitoring mode(MRM).The analysis of 15 illicit drugs could be completed within 10 minutes,and the ion chromatograms of each component had good peak shape and retention time between 2.21 and 7.76 min.The correlation coefficient of each component in the linear range of 5-100μg/L was greater than 0.99,the detection limit was 32.5-60.6μg/kg,the quantification limit was 97.5-157.5μg/kg,and the recovery rates of 15 prohibited drugs at three spiked concentrations(80μg/kg,40μg/kg,20μg/kg)were 78.8%-118.8%with the relative standard deviations less than 10%(n=6).This method has the advantages of simple operation,rapid analysis,and low matrix interference,and is suitable for the screening of various aphrodisiac drugs in wolfberry wine.

关 键 词：超高效液相色谱-串联质谱法 枸杞酒 违禁药物 快速筛查 

分 类 号：O657.63[理学—分析化学] TS218[理学—化学]