超高效液相色谱-荧光法测定丹参饮片中黄曲霉毒素  

Determination of aflatoxin in Salvia miltiorrhiza pieces by ultra performance liquid chromatography-fluorescence detection

作　　者：潘超 李海燕 岳洪水 鞠爱春 PAN Chao;LI Haiyan;YUE Hongshui;JU Aichun(Tianjin Tasly Pride Pharmaceutical Co.,Ltd.,Tianjin 300410,China;Tianjin Key Laboratory of Advanced Technology Enterprise of TCM Injections,Tianjin 300410,China)

机构地区：[1]天津天士力之骄药业有限公司,天津300410 [2]天津市中药注射剂安全性评价企业重点实验室,天津300410

出　　处：《药物评价研究》2021年第11期2419-2423,共5页Drug Evaluation Research

摘　　要：目的建立超高效液相色谱-荧光法测定丹参饮片中黄曲霉毒素B_(1)、B_(2)、G_(1)、G_(2)。方法样品经70%甲醇提取,通过免疫亲和柱净化后,用超高效液相色谱-荧光法进行分析测定,WatersAcquityUPLC BEHC_(18)色谱柱(100mm×2.1mm,1.7μm);流动相为甲醇-乙腈(1∶1)、水,梯度洗脱;体积流量0.4 mL/min;柱温30℃;荧光检测器激发波长365 nm;发射波长456 nm;进样量2μL。结果黄曲霉毒素B_(1)、B_(2)、G_(1)、G_(2)分别在0.1201~1.9208、0.0361~0.5772、0.1221~1.9540、0.0421~0.6732 ng/mL内线性关系良好,r均大于0.99;定量限分别为0.10、0.03、0.39、0.03 ng/mL;黄曲霉毒素B_(1)的回收率为107%,RSD为6%;黄曲霉毒素总含量的回收率为80%,RSD为9%。专属性、重复性、精密度、稳定性试验均符合检测要求。结论所建立的方法准确、可靠、专属性强,可准确地测定丹参饮片中黄曲霉毒素的含量。Objective To establish an ultra performance liquid chromatography-fluorescence detection method for determination of aflatoxin B_(1),B_(2),G_(1),G_(2) in Salvia miltiorrhiza pieces.Methods After being extracted by 70%methanol solution and purification by immune affinity columns,aflatoxin B_(1),B_(2),G_(1),G_(2) were analyzed by ultra performance liquid chromatography-fluorescence detection.Chromatographic conditions were as follows:Acquity UPLC BEH C_(18) column(100 mm×2.1 mm,1.7μm),the mobile phase consisted of methanol-acetonitrile(1∶1)and water with gradient elution,volume flow was 0.4 mL/min,column temperature was 30℃,excitation wavelength of fluorescence detector was 365 nm;the emission wavelength was 456 nm;injection volume was 2μL.Results Aflatoxin B_(1)showed a good linear relationship at a range of 0.1201—1.9208 ng/mL,a-flatoxin B_(2)at a range of 0.0361—0.5772 ng/mL,aflatoxin G_(1) at a range of 0.1221—1.9540 ng/mL and aflatoxin G_(2) at a range of 0.0421—0.6732 ng/mL,r≥0.99.The quantitation limits are 0.10,0.03,0.39,0.03 ng/mL.The recovery of aflato-xin B_(1) was 107%and RSD was 6%.The recovery of total aflatoxin content was 80%and RSD was 9%.The specificity,repeatability,precision and stability tests all meet the testing requirements.Conclusion The established method is accurate,reliable and specific,it can accurately determine the content of aflatoxin in Salvia miltiorrhiza pieces.

关 键 词：丹参饮片 超高效液相色谱-荧光检测法(UPLC-FLR) 黄曲霉毒素B_(1) 黄曲霉毒素B_(2) 黄曲霉毒素G1 黄曲霉毒素G2 

分 类 号：R284.1[医药卫生—中药学]