UHPLC-MS/MS同时测定活血化瘀类中成药中非法添加的30个化学药物

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维普

中文摘要：目的建立超高效液相色谱-串联质谱法同时测定活血化瘀类中成药中非法添加抗心绞痛、抗凝、抗血小板聚集以及抗炎镇痛等30个化学药物的方法。方法样品采用60％甲醇超声提取，以0。1％甲酸溶液-乙腈为流动相进行梯度洗脱，经色谱柱Phenomenex Kinetex C18(2。1 mm×100 mm，2。6 μm)分离，流速为0。3 mL·min-1，柱温为40 ℃。质谱采用电喷雾电离，正负离子同时扫描，多反应监测的模式采集数据。结果 30个化合物在考察的浓度范围内线性关系良好，相关系数均＞0。999，各化合物的检出限为1。3～238。4 ng·g-1，平均回收率为63。7％～108。2％，RSD为1。0％～6。7％。采用该方法对90批舒筋活血片进行检测，共有3批检出对乙酰氨基酚，其余化合物均未检出。对乙酰氨基酚检出量为每片0。16～0。93 μg，远低于对应药品日服用的最小剂量，排除人为故意添加。可能的原因是企业共线生产清洁验证不彻底引起的残留。结论该方法快速准确，灵敏度高，高选择性，可用于活血化瘀类中成药非法添加30个化合物的定性筛查和定量检测。

外文标题：Simultaneous Determination of 30 Compounds Illegally Added in Chinese Patent Medicine for Promoting Blood Circulation and Removing Blood Stasis Medicine by UHPLC-MS/MS

外文摘要：OBJECTIVE To establish an ultra-performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of 30 compounds(including antianginal drugs,anticoagulant,anti-platelet aggregators and anti-inflammatory analgesics)illegally added in Chinese patent medicine for promoting blood circulation and removing blood stasis.METHODS The sample was extracted by ultrasonication with 60％ methanol.The analysis was performed on Phenomenex Kinetex C18 column(2.1 mm× 100 mm,2.6 μm)with gradient elution using 0.1％ formic acid solution and acetonitrile as the mobile phase at the flow rate of 0.3 mL·min-1,and the column temperature was 40 ℃.Mass spectrometry was collected using electrospray ionization(ESI),simultaneous scanning of positive and negative ions,and multiple reaction monitoring mode.RESULTS The linearity of the 30 compounds was good in the mass range examined,with the correlation coefficients all＞0.999.The limits of detection of each compound ranged from 1.3 to 238.4 ng·g-1 and the average recoveries ranged from 63.7％ to 108.2％with the RSDs of 1.0％ to 6.7％.The method was used to test 90 batches of Shujin Huoxue tablets.Paracetamol was detected in 3 batches,while the rest of the compounds were not detected.The amount of paracetamol detected ranged from 0.16 to 0.93 μg per tablet,which was much lower than the minimum daily dose of the corresponding drug,excluding intentional addition.The probable explanation was the residues caused by incomplete cleaning validation of the enterprise's collinear production.CONCLUSION This method is rapid,accurate,highly sensitive,and highly selective,and can be used for qualitative screening and quantitative determination of 30 chemical compounds illegally added in Chinese patent medicine for promoting blood circulation and removing blood stasis.

外文关键词：

promoting blood circulation and removing blood stasisShujin Huoxue tabletsillegally addedantianginal drugsanticoagulantanti-platelet aggregatorsanti-inflammatory analgesicsUHPLC-MS/MS

作者：

张琳琳、李正、杨欢、郑成、唐登峰、陈碧莲

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作者单位：

浙江省食品药品检验研究院,国家药品监督管理局中成药质量评价重点实验室,杭州 310052

关键词：

活血化瘀舒筋活血片非法添加抗心绞痛药抗凝药抗血小板药抗炎镇痛药超高效液相色谱-串联质谱法

基金：

浙江省科技计划浙江省中医药科技计划浙江省中医药科技计划浙江省药品监督管理局科技项目

项目编号：

2021C020192023ZF1302021ZB1782023007

出版年：

2024

DOI：

10.13748/j.cnki.issn1007-7693.20222257

中国现代应用药学

中国药学会

中国现代应用药学

CSTPCD北大核心

影响因子：0.877

ISSN：1007-7693

年,卷(期)：2024.41(3)

参考文献量21