LC-MS检测硫酸亚铁缓释片中邻苯二甲酸二辛酯含量

Quantitative Determination of Dioctyl Phthalate(DOP) in Ferrous Sulfate Sustained Release Tablets by LC-MS

关键词:  液相色谱-质谱联用  多反应监测  硫酸亚铁缓释片  邻苯二甲酸二辛酯

Key words:  LC-MS  multiple reaction monitoring  ferrous sulfate sustained release tablets  dioctyl phthalate

摘要:

目的 建立液-质联用(LC-MS)法检测硫酸亚铁缓释片中邻苯二甲酸二辛酯(DOP)的含量。方法 采用Waters BEH C₁₈(50 mm×2.1 mm，1.7 μm)色谱柱，流动相为95%甲醇-5%乙酸铵溶液梯度洗脱，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)，两通道391→149，391→167。结果 DOP在0.091 3~0.913 0 ng内线性关系良好，回归方程为Y=268 462X+162 526(r=0.997 3)；以加标样品计算，在低、中、高3个浓度水平下，DOP平均回收率为98.5%；定量限为0.05 ng，检测限为0.01 ng。结论 本方法灵敏度高，结果准确可靠，适用于硫酸亚铁缓释片中DOP的含量检测。

Abstract:

OBJECTIVE To establish a method for the quantitative determination of DOP in ferrous sulfate sustained release tablets by LC-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 95% methanol-5% ammonium acetate water solution(gradiently eluting) as mobile phase at a flow rate of 0.2 mL·min^-1. Determination was performed by multiple reaction monitoring mode in two channels, 391→149, 391→167, using electrospray ionization in positive ion mode. RESULTS DOP had a good linear relationship in 0.0913-0.9130 ng with the linear regression equation Y=268 462X+162 526(r=0.997 3). The recovery of DOP evaluated by determining the spiked samples at low, medium and high concentrations was 98.5%. The limits of quantitation and detection were 0.05 ng and 0.01 ng, respectively. CONCLUSION The method was sensitive and accurate which could be an appropriate technique to detect the DOP in ferrous sulfate sustained release tablets.