跌打丸中黄曲霉毒素的测定及安全性评价  

Determination and safety evaluation of aflatoxins in Dieda Pills

作　　者：于洲 孙慧珠 刘永利 YU Zhou;SUN Huizhu;LIU Yongli(Shijiazhuang No.4 Pharmaceutical,Shijiazhuang 052100,China;Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050227,China)

机构地区：[1]石家庄四药有限公司,河北石家庄052100 [2]河北省药品医疗器械检验研究院,河北石家庄050227

出　　处：《药学研究》2021年第8期504-507,共4页Journal of Pharmaceutical Research

摘　　要：目的对跌打丸中黄曲霉毒素G_( 2)、G_( 1)、B_( 2)、B_( 1)进行测定,并评价跌打丸中黄曲霉毒素安全性。方法采用超高效液相色谱质谱联用(UPLC/MS/MS)法,C_(18)色谱柱(2.1 mm×100 mm,1.7μm),流动相为甲醇-10 mmol·L^(-1)醋酸铵溶液,梯度洗脱,电喷雾离子源(ESI+),多反应监测(MRM)模式。对全国流通领域抽取的76批样品进行测定,评价其安全性。结果黄曲霉毒素B_( 1)、G_( 1)在0.06~10 ng·mL^(-1),B 2、G 2在0.02~3 ng·mL^(-1)范围内线性良好;平均回收率分别为98.2%、100.9%、88.2%、94.8%,RSD均小于5.0%。76批样品中有1个企业的3批样品检出黄曲霉毒素G_( 1)、B _(1),但未超过限度,其余73批均未检出。结论建立的方法快速简便,可准确地分析跌打丸中黄曲霉毒素含量,样品测定结果表明跌打丸中黄曲霉毒素污染风险小。Objective To determine aflatoxin B_( 1),B_( 2),G_( 1) and G_( 2) in Dieda Pills by UPLC/MS/MS and evaluate the safety.Methods The product was analyzed by UPLC/MS/MS using a C_(18) column(2.1 mm×100 mm,1.7μm)with methanol-10 mmol ammonium acetate as mobile phase for gradient elution.Electrospray ion source(ESI^(+)),multi-reaction monitoring(MRM)mode.The 76 batches of sample from nation-wide market were detected by the method.Results Linear relationships were obtained within the range of 0.06~10 ng·mL^(-1) for aflatoxin B_( 1 )and G_( 1),and 0.02~3 ng·mL^(-1) for aflatoxin B_( 2 )and G_( 2).The recoveries of aflatoxin B_( 1),B_( 2),G_( 1) and G_( 2) were 98.2%,100.9%,88.2%and 94.8%,respectively,with all the RSD below 5.0%.Aflatoxin G_( 1 )and B_( 1 )were detected in 3 batches of samples from the same company among 76 batches,but the content were not exceed the limit.The other 73 batches were not detected.Conclusion The developed method was convenient and accurate,and the results showed that the risk of aflatoxin contamination was low.

关 键 词：跌打丸 黄曲霉毒素 安全性评价 

分 类 号：R927.1[医药卫生—药学]