固相萃取净化-UPLC-MS/MS法同时测定中成药及保健食品中添加的17个抗过敏类化学成分

目的：建立了固相萃取柱净化，超高效液相色谱-三重四极杆串联质谱联用（UPLC-MS/MS）测定中成药及保健食品中添加的17个抗过敏类化学成分的方法。方法：样品用甲醇提取后，与2%甲酸溶液以1∶9的比例混合，经Oasis MCX固相萃取柱净化，采用Waters ACQUITY UPLC BEH C₁₈（2.1 mm×100 mm，1.8 μm）分离16个化学成分，以甲醇-0.1%氨水为流动相进行梯度洗脱；大赛璐CHIRALPAK AGP柱（150 mm×4 mm，5 μm）分离2个手性化学成分（西替利嗪与左西替利嗪），以甲醇-10 mmol·L^-1乙酸铵（v/v）溶液为流动相等度洗脱。在电喷雾离子源（ESI）正负离子模式下电离，多反应监测（MRM）模式下测定。结果：17个抗过敏化学成分在相应的测定范围内线性关系良好，相关系数（r）在0.995 7~1.000之间，在3个加标水平下，加标回收率范围为84.3%~112.9%，RSD（n=6）为0.43%~3.7%，各化学成分的检测下限在0.14~0.91 mg·kg^-1之间。收集的32批次样品中5批次检出氯苯那敏，含量在0.015~3.86 mg·g^-1之间、1批次检出西替利嗪，含量为1.68 mg·g^-1，1批次检出左西替利嗪，含量为1.93 mg·g^-1，1批次检出苯海拉明，含量为1.30 mg·g^-1。结论：该方法简便，选择性好，灵敏度高，可用于中成药和保健食品中多组分抗过敏类化学成分的同时定量测定。

Objective:To develop a method based on SPE-UPLC-MS/MS(solid phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry)for determination of 17 anti-allergic chemical components in Chinese patent medicine and health foods.Methods:Samples were extracted with methanol and then mixed with 2% formic acid solution at a ratio of 1:9 in volume before purification with an Oasis MCX column.16 componewts were separated on an ACQUITY UPLC BEH C₁₈(2.1 mm×100 mm,1.8 μm)column with 0.1% ammonia-methanol as mobile phases by gradient elution.A CHIRALPAK AGP(150 mm×4 mm, 5 μm)column and gradient elution of 10 mmol·L^-1 ammonium acetate and methanol were applied to separate two kinds of chiral components(cetirizine and levocetirizine).Detection was carried out by positive and negative electrospray ionization(ESI)mass spectrometer in multiple reaction monitor(MRM)mode.Results:All the 17 anti-allergic chemical components showed good linearity in their reasonable ranges(r=0.995 7-1.000).The average recoveries of all the componewts at three spiked levels were in the range of 84.3%-112.9% with RSDs(n=6)within 0.43%-3.7%.The LODs were all in the range of 0.14-0.91 mg·kg^-1.Chlorpheniramine was found in 5 of the 32 tested samples,the contents were in range of 0.015-3.86 mg·g^-1.Cetirizine and levocetirizine were found in 1 batch(cetirizine:1.68 mg·g^-1,levocetirizine:1.93 mg·g^-1).In another sample,diphenhydramine was detected(1.30 mg·g^-1).Conclusion:With the advantages of rapidness,simplicity,good selectivity and high sensitivity,the method can be used in determination of anti-allergic compounds in Chinese patent medicine and health foods.

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