高效液相色谱-串联质谱法同时测定凉茶中5种α-受体阻断剂  

Simultaneous Determination of 5 Kinds of a-receptor Antagonists in Herbal Tea by High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：周铭林 何海彤 曾芷琳 ZHOU Minglin;HE Haitong;ZENG Zhilin(Guangdong Testing Institute of Product Quality Supervision;Guangdong Pharmaceutical University)

机构地区：[1]广东产品质量监督检验研究院 [2]广东药科大学

出　　处：《中国食品安全》2024年第2期61-66,共6页CHINA FOOD SAFETY

摘　　要：目的:建立高效液相色谱-串联质谱法同时测定凉茶中5种α-受体阻断剂。方法:样品经过甲醇提取,结合MCX固相萃取柱净化,采用Waters ACQUITY UPLC(BEH C_(18) 1.7μm)色谱柱分离,在甲酸水(0.1%)和乙腈溶液为流动相条件下进行梯度洗脱,采用多反应监测正离子模式(ESI~+),实现对酚妥拉明、哌唑嗪、特拉唑嗪、育亨宾、妥拉唑林共5种α-受体阻断剂的定性定量(外标法)分析。结果:该方法分析时间适中,5种组分均可分离完全,线性良好,相关系数均大于0.994,定量限为0.005 mg/kg~0.04 mg/kg,在0.005 mg/kg~0.4 mg/kg加标范围内,平均回收率(n=6)为70.9%~96.3%,相对标准偏差为0.92%~3.98%。结论:建立的高效液相色谱-串联质谱法满足同时检测凉茶中5种α-受体阻断剂的要求,该方法操作简单,分析时长短,可批量检测,精密度高,重复性好。Objective:To establish a method for determination of 5 kinds of a-receptor antagonists residues in herbal tea by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Method:The sample was extracted by methanol and purified by MCX solid-phase extraction column.The components were separated on Waters ACQUITY UPLC(BEH C181.7μm)chromatographic column.Gradient elution was carried out under the mobile phase of formic acid water(0.1%)and acetonitrile solution.Five kinds ofα-receptor antagonists such as phentolamine,tolazoline,prazosin,terazosin and yohimbine were qualitatively and quantitatively determined with positive ion mode with multiple reactions(external standard method).Results:The analytical time of this method was moderate;The 5 components could be separated completely,and the linearity was good.The correlation coefficients were all greater than 0.994 and the limits of quantitative(S/N=10)were 0.005~0.04 mg/kg;The average recoveries(n=6)were 70.9%~96.3%in the spiked range of 0.005~0.4 mg/kg,and the relative standard deviations(RSD%)were 0.92%~3.98%.Conclusion:The established HPLC-tandem mass spectrometry method meets the requirement of simultaneous detection of 5 kinds ofα-receptor antagonists in herbal tea.The method is simple in operation,rapid in analyst,high precision and good repeatability.

关 键 词：分析化学 凉茶 高效液相色谱-串联质谱法 Α-受体阻断剂 

分 类 号：O65[理学—分析化学]