UPLC-MS/MS检测小儿咳喘灵颗粒中4种黄曲霉毒素及灰毡毛忍冬皂苷乙  

Detection of Four Aflatoxins and Macranthoidin B in Xiaoer Kechuanling Granules by UPLC-MS/MS

作　　者：石慧君 张文丽 SHI Huijun;ZHANG Wenli(Jiujiang Center of Inspection and Certification,Jiujiang Jiangxi 332000,China)

机构地区：[1]九江市检验检测认证中心,江西九江332000

出　　处：《药品评价》2022年第13期773-779,共7页Drug Evaluation

摘　　要：目的:分别建立小儿咳喘灵颗粒中黄曲霉毒素 B_(1)、B_(2)、G_(1)、G_(2)及灰毡毛忍冬皂苷乙的 UPLC-MS/MS 测定方法,以期将小儿咳喘灵颗粒检验标准提升。方法:两者均采用 UPLC-MS/MS 法,色谱柱均为 UPLC ACQUITY BEH(100mm×2.1 mm,1.7 μm)。样品经免疫亲和柱前处理,以乙腈 -0.2% 甲酸溶液为流动相,采用 MRM 扫描、ESI+ 模式,选择 4 种黄曲霉毒素,成分响应最佳的质谱参数测定;灰毡毛忍冬皂苷乙以乙腈 -0.1% 甲酸溶液作为流动相,采用 MRM扫描、ESI- 模式,优化质谱参数测定。结果:黄曲霉毒素 B_(1)、B_(2)、G_(1)和 G_(2)各自在 0.186~9.300 ng/m L、0.060~3.000 ng/m L、0.186~9.300 ng/m L、0.070~3.500 ng/m L 检测范围内线性良好,r ≥ 0.995 9;加样回收率在 81.2%~91.9%;样品中 4种黄曲霉毒素浓度均低于检测限。灰毡毛忍冬皂苷乙在 0.083~2.501 ng 检测范围内线性良好,r=0.999 0;加样平均回收率为 100.9%;有 3 批样品检出。结论:基于 UPLC-MS/MS 建立的两种方法定性定量快速、准确,能有效提高小儿咳喘灵颗粒检验标准。Objective:To develop UPLC-MS/MS methods to determine aflatoxin B_(1),B_(2),G_(1),G_(2) and macranthoidin B,respectively.And help improve the inspection standard of xiaoer kechuanling granules.Methods:Both methods were performed by UPLC-MS/MS system with UPLC ACQUITY BEH(100 mm×2.1 mm,1.7 μm)column.4 aflatoxins in xiaoer kechuanling granules were pretreated with immunoaffinity column,acetonitrile and water (0.2% formic acid) were used as mobile phase,MRM mode was adopted and ESI positive source was used.The four compounds responded highly by optimizing MS parameters;detemination of macranthoidin B in Xiaoer kechuanling granules use acetonitrile and water (0.1%formic acid) as mobile phase,MRM mode was adopted and ESI negative source was used.Optimum MS parameters were selected.Results:The linear range of aflatoxin B_(1),B_(2),G_(1) and G_(2) was 0.186-9.300 ng/m L,0.060-3.000 ng/m L,0.186-9.300ng/m L,0.070-3.500 ng/m L,respectively,r ≥ 0.995 9;the recovery was 81.2%-91.9%;the concentrations of 4 aflatoxins in the samples were lower than limit of detection.The linear range of macranthoidin B was 0.083-2.501 ng,r=0.999 0;the average recovery was 101.0%;3 batches of samples were positive.Conclusion:The two methods established based on UPLC-MS/MS were rapid and accurate in qualitative and quantitative analysis,and could effectively improve the inspection standard of xiaoer kechuanling granules.

关 键 词：UPLC-MS/MS 小儿咳喘灵颗粒 黄曲霉毒素 灰毡毛忍冬皂苷乙 

分 类 号：R286.0[医药卫生—中药学]