降压类中成药及保健食品中非法添加氯沙坦的定性定量检测方法研究

摘要

Objective To establish a qualitative and quantitative method for the detection of losartan illegally added into antihypertensive traditional Chinese medicines and health food. Methods Qualitative screening of losartan illegally added into antihypertensive traditional Chinese medicine and health food was firstly performed by UPLC-Q-TOF-MS/MS. The qualitative analysis was performed on a Shi-madzu Shim-pack XR-ODS column(100 mm × 2. 0 mm,2. 2 μm) with the mobile phase of acetonitrile and 0. 5% formic acid by gradient elution,the flow rate was 0. 3 mL/min. Electrospray ionization source(ESI) was operated in positive and negative mode. The scan range was from 100 to 1 000 m/ z. The quantitative detection of positive sample detected by UPLC-Q-TOF-MS/MS was used by HPLC,Chromatographic separation was achieved on a Waters XBridgeTM C18 column (150 mm × 4. 6 mm,5 μm) with the mobile phase of acetonitril and 0. 2% phosphate by gradient elution. The detection wavelengths was 220 nm and the flow rate was 1. 0 mL/min. Results Sampling from the market in 9 batches of Chinese patent medicines and health food diet,there were 2 batch samples detected illegally added losartan. The losartan content was 48. 3,20. 9 mg/g. Conclusion The method is rapid,accurate and highly sensitive, which can be used as a supplementary test method of antihypertensive traditional Chinese medicines and health food illegally added losartan.%目的：建立降压类中成药及保健食品中非法添加氯沙坦的定性及定量检测方法。方法采用超高效液相色谱－四级杆－飞行时间串联质谱（UPLC－Q－TOF）联用技术对降压类中成药及保健食品中非法添加的氯沙坦进行定性筛查，采用Shimadzu Shim－pack XR－ODS色谱柱（100 mm ×2.0 mm，2.2μm），以0.5%甲酸溶液－乙腈为流动相进行梯度洗脱，流速为0.3 mL／min，电喷雾离子源( ESI )，正负离子检测，扫描范围 m／ z 100～1000。经筛查为阳性的样品用超高效液相色谱进行紫外吸收光谱定性鉴别和定量测定，采用Wa-ters XBridgeTM色谱柱（150 mm ×4.6 mm，5μm），以0.2%磷酸溶液－乙腈为流动相进行梯度洗脱，检测波长为220 nm，流速为1.0 mL／min。结果通过对9批降压类中成药和保健食品进行快速质谱定性筛查，有2批样品检出氯沙坦，含量分别为48.3，20.9 mg／g。结论该方法准确性好、灵敏度高、选择性强，可作为降压类中成药及保健食品中非法添加氯沙坦的检验方法。