LC-MS/MS法快速分析保健食品中非法添加的11种降压类化学成分

Rapid Analysis of 11 Antihypertensive Chemical Components Illegally Added in Health Food by LC-MS/MS Method

目的:建立液相色谱串联质谱(Liquid Chromatograph Tandem Mass Spectrometer,LC-MS/MS)法快速分析保健食品中非法添加的11种降压类化学成分的方法。方法:采用Kinetex 2.6μm Phenyi-Hexyi 100Å(100 mm×2.1 mm,5.0μm)色谱柱进行分离,以0.01%甲酸水-乙腈为流动相梯度洗脱,流速为0.4 mL·min^(-1),离子源为ESI,正负离子检测模式,对降压类保健食品中非法添加的11种化学成分进行定性定量检测。结果:11种化学成分在1.0~250.0 ng·mL^(-1)线性关系良好,相关系数(r)均大于0.997,检出限在0.0042~0.1700 ng·g^(-1),定量限在0.013~0.520 ng·g^(-1),在0.20μg·g^(-1)、1.25μg·g^(-1)和10.00μg·g^(-1)3个加标水平下的回收率分别为74.9%~118.8%、82.1%~116.0%、93.5%~106.3%,连续6针精密度为1.3%~9.9%,日内精密度为1.9%~14.5%。结论:该方法操作容易,结果准确,适用于降压类保健食品中非法添加硝苯地平等11种化学成分的定性定量分析。

Objective:To establish a rapid method for the analysis of 11 antihypertensive chemical components illegally added in health food by liquid chromatograph tandem mass spectrometer(LC-MS/MS).Method:The separation was performed on Kinetex 2.6μm Phenyi-Hexyi 100Å(100 mm×2.1 mm,5.0μm)column,and gradient elution was performed on 0.01%formic acid-acetonitrile as mobile phase at the flow rate of 0.4 mL·min^(-1).The ion source was ESI and the positive and negative ion detection mode was adopted.Qualitative and quantitative detection of 11 chemical components illegally added in antihypertensive health food was carried out.Result:The linear relationship between the 11 chemical components was good in the range of 1.0 ng·mL^(-1)to 250.0 ng·mL^(-1),the correlation coefficient(r)was greater than 0.997,the detection limit was 0.0042~0.1700 ng·g^(-1),and the quantitation limit was 0.013~0.520 ng·g^(-1).At 0.20μg·g^(-1),1.25μg·g^(-1)and 10.00μg·g^(-1),the recoveries were 74.9%~118.8%,82.1%~116.0%and 93.5%~106.3%,respectively.The precision of 6 consecutive needles was 1.3%~9.9%.The intraday precision is 1.9%~14.5%.Conclusion:The method is easy to operate,accurate and suitable for qualitative and quantitative analysis of 11 chemical components such as nifedipine illegally added in antihypertensive health food.