保健胶囊中磷脂酰胆碱的UPLC检测及质谱确证

Phosphatidylcholine in Health Supplement Capsules Detected by Ultra-performance Liquid Chromatography and Verified by Mass Spectrometry

摘要:

建立了保健胶囊中磷脂酰胆碱的超高效液相色谱（UPLC）测定和超高效液相色谱-质谱/质谱（UPLC-MS/MS）确证方法。样品经直接稀释或液液分配除杂，采用BEH HILIC色谱柱分离，以甲醇和异丙醇为流动相进行等度洗脱，二极管阵列（PDA）检测器进行定量分析，采用UPLC-MS/MS电喷雾离子源正离子（ESI+）-多反应监测（MRM）模式进一步确证。仪器检出限为0.001 mg/mL，线性范围在0.005 mg/mL到0.100 mg/mL之间。采用阴性大豆油进行添加回收实验，6个浓度水平的平均添加回收率为83.3%，平均相对标准偏差为4.5%。用该方法测定标示值为11.4 g/100 g的保健胶囊样品，平行测定检测结果分别为8.93 g/100 g和8.76 g/100 g，相对标准偏差3.02%和0.60%。结果表明，该方法准确，快速，适用于保健胶囊中磷脂酰胆碱的检测和确证。

Abstract:

A new method was established to detect phosphatidylcholine in health supplement capsules, using ultra-performance liquid chromatography (UPLC) and the result was further verified using UPLC-tandem mass spectrometry (UPLC-MS/MS). The capsule contents were diluted before being tested or went through liquid-liquid-partitiondepuration. The analytes were separated using a BEH HILIC column and isocratic elution with methanol and isopropanol as the mobile phase. The analyte quantitates were detected by a photodiode array (PDA) detector and further verified by UPLC-MS/MS operated using electrospray ionization cation (ESI+)-muti-reaction monitoring( MRM). The detection limit was 0.001 mg/mL and linear range was between 0.005 and 0.100 mg/mL. The mean addition recovery rate of 6 concentrations was 83.3%, with a mean, relative standard deviation of 4.5%. Health supplement capsule marked 11.4 g/100 g was tested using this method with parallel determination results of 8.93 g/100 g and 8.76 g/100 g and the relative standard deviation of 3.02% and 0.60%, respectively. The results showed that the method is accurate, fast, and suitable for the determination and verification of phosphatidylcholine in health supplement capsules.