摘要
取2.00 g样品置于50 mL具塞离心管中,加入10 mL提取剂[片剂、胶囊、粉末和口服液样品提取剂为乙腈;保健酒样品提取剂为体积比60∶39∶1的乙腈-水-甲酸混合溶液;软凝胶、保健茶叶样品提取剂为60%(体积分数)甲醇溶液],涡旋混匀,振荡30 min,于4℃以转速3500 r·min^(-1)离心3 min,取上清液于40℃氮气吹至近干,加入1 m L提取剂涡旋溶解30 s,过0.22μm尼龙滤膜,采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法(UHPLC-Q-Orbitrap HRMS)分析滤液中97种化学药物。以Hypersil GOLD色谱柱为固定相,以不同体积比的含0.1%(体积分数)甲酸的甲醇溶液-2.0 mmol·L^(-1)乙酸铵溶液混合溶液为流动相进行梯度洗脱,质谱分析采用加热电喷雾离子(HESI)源,一级质谱全扫描(Full MS)模式下的分辨率为70000,离子注入时间(IT)为100 ms;数据依赖的二级质谱扫描(dd-MS2)模式下的分辨率为17500,IT为50 ms。结果表明,97种化学药物在固体基质(片剂、胶囊、粉末)、口服液、保健酒、保健茶叶和软凝胶中的检出限分别为1.22~68.20μg·kg^(-1),2.25~101.41μg·kg^(-1),1.38~39.80μg·kg^(-1),2.70~93.52μg·kg^(-1),2.50~71.76μg·kg^(-1)。方法用于50个保健品的分析,其中5个样品中检出苯丙酸诺龙、乙酸甲羟孕酮、扑热息痛和美伐他汀。
2.00 g of the sample was taken,and placed in a 50 mL-stoppered centrifuge tube.10 mL of extraction agent was added[extraction agent for tablet,capsule,powder,and oral liquid samples was acetonitrile,extraction agent for health wine samples was a mixture of acetonitrile-water-formic acid at a volume ratio of 60∶39∶1,and extraction agent for soft gel and health tea samples was 60%(volume fraction)methanol solution].The mixture was vortex mixed,shaken for 30 min and centrifuged at a rotational speed of 3500 r·min^(−1) for 3 min at 4℃.The supernatant was taken,and blown to near dryness by nitrogen at 40℃.1 mL of extraction agent was added,and the mixture was vortex dissolved for 30 s.The solution was passed through a 0.22μm nylon filter membrane,and the 97 chemical drugs in the filtrate was analyzed by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UHPLC-Q-Orbitrap HRMS).Hypersil GOLD chromatographic column was used as the stationary phase and the mixed solution composed of methanol solution containing 0.1%(volume fraction)formic acid and 2.0 mmol·L^(−1) ammonium acetate solution at different volume ratios was used as the mobile phase for gradient elution.Heating electrospray ion(HESI)source was used for mass spectrometry.The resolution was set to 70000 and the ion implantation time(IT)was 100 ms in primary mass spectrometry full scan(Full MS)mode,while the resolution was set to 17500 and the IT was 50 ms in the data dependent secondary mass spectrometry scanning(dd-MS2)mode.As shown by the results,the detection limits of 97 chemical drugs in solid matrix(tablet,capsule,and powder),oral liquid,health wine,health tea and soft gel were in the ranges of 1.22-68.20μg·kg−1,2.25-101.41μg·kg−1,1.38-39.80μg·kg−1,2.70-93.52μg·kg−1,and 2.50-71.76μg·kg−1,respectively.This method was used for the analysis of 50 samples of health product,and nandrolone phenylpropionate,medroxyprogesterone acetate,acetaminophen,and mevastatin in 5 samples were detected.
作者
燕传勇
郑佳
马璐瑶
郗存显
郭思言
张文华
母昭德
YAN Chuanyong;ZHENG Jia;MA Luyao;XI Cunxian;GUO Siyan;ZHANG Wenhua;MU Zhaode(China University of Mining and Technology,Xuzhou 221004,China;Xuzhou College of Industrial Technology,Xuzhou 221140,China;College of Pharmacy,Chongqing Medical University,Chongqing 400016,China;Research Center for Pharmacodynamic Evaluation Engineering Technology of Chongqing,Chongqing 400016,China;Chongqing Customs Technology Center,Chongqing 400020,China;Technical Center of Hangzhou Customs,Hangzhou 310016,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2024年第11期1173-1182,共10页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
海关总署科研项目(2020HK196,2021HK206)。
