UPLC-MS/MS测定延时类保健品中三种局麻药的含量

Quantitative Determination of Three Local Anesthetics in Delay Drugs by UPLC-MS/MSHUANG Zhaohui1, CAI Dandan2, CHEN Zhongyi1, ZHUO Kaihua1 (1 Ningbo Institute for Drug Control, Ningbo 315048, China;2 Ningbo Drug Research Center, Ningbo 315010, China;)

关键词:  超高效液相-质谱联用  多反应监测  局麻药

Key words:  UPLC-MS/MS  multiple reaction monitoring  local anesthetics  

摘要:

目的 建立一种测定延时类保健品中三种局麻药含量的超高效液相-质谱联用方法。方法 采用Waters BEH C₁₈(50 mm?2.1 mm,1.7 μm)色谱柱,流动相为含0.1%乙酸的0.02 mol.L_-1乙酸铵溶液-乙腈(72:28),流速为0.2 mL.min_-1,柱温为35℃；质谱采用电喷雾离子源,多反应监测模式(正离子)。结果 三种局麻药在20 μg.L_-1～200μg.L_-1内线性关系良好,r值为0.9988～0.9998之间,平均回收率为98.2%～101.2%之间,分析方法的定量下限为0.5μg.L_-1,检测限为0.1μg.L_-1。结论 该方法分析速度快,灵敏度高,结果准确可靠,适用于延时类保健品中局麻药的测定,为打击保健品非法添加提供了有力的技术手段。

Abstract:

ABSTRACT: OBJECTIVE To establish a method for the quantitative determination of 3 local anesthetics in delay drugs by UPLC-MS/MS. METHODS Chromatography was carried on a Waters BEH C18 column(50 mm×2.1 mm, 1.7 μm) with the column temperature at 35 ℃, using 0.02 mol?L-1 ammonium acetate water solution(containing 0.1% acetic acid) -acetonitril (72:28) as mobile phase at a flow rate of 0.2 mL?min-1. Determination was performed by multiple reaction monitoring mode using electrospray ionization in positive ion mode. RESULTS Three chemical medicines had good linear relationships in 20 μg?L-1-200 μg?L-1 (r=0.9988-0.9998). average recovery were 98.2%-101.2%.The limits of quantitation and detection were 0.5 μg?L-1 and 0.1 μg?L-1, respectively. CONCLUSION The method is rapid, sensitive and accurate, and could be an appropriate technique to detect the local anesthetics in delay drugs.