摘要
建立免疫亲和柱净化-快速液相色谱-串联质谱法测定江西市场26味中药中4种黄曲霉素(B_1、B_2、G_1和G_2)。样品经甲醇-水(70∶30,V/V)提取离心后,用免疫亲和柱净化、浓缩,Luna C18(2)100柱(150×2.0mm i.d.,3μm)分离,以甲醇-5mmol/L乙酸铵水溶液(含0.1%甲酸)(1∶1)为流动相,流速0.3mL/min,进样量1μL,电喷雾正离子模式(ESI^+),多反应监测(MRM)模式扫描,外标法定量。4种黄曲霉毒素均在0.6~30.0ng范围内呈良好线性,相关系数R^2分别为0.99997、0.99904、0.99961、0.99999,加标回收率为73.8%~100.8%。本法快速、准确、灵敏、精密度高、专属性强,可实现中药中黄曲霉毒素的测定和确证。
An immunoaffinity column（IAC）clean-up rapid resolution liquid chromatography（RRLC）MS/MS method was developed for determining 4 aflatoxins B1,B2,G1 and G2 in twenty-six traditional Chinese medicines.Samples were extracted with mixed solvents of methanol and water（70∶30,V/V）,the extracts were centrifuged,cleaned-up and concentrated with IAC,then the target compounds were eluted by methanol and injected with 1μL volume into liquid chromatography-tandem mass spectrometry.The separation of target compounds was performed on a Luna C18（2）100column（150×2.0 mm i.d.,3μm）at 30℃ with methanol and 5 mmol/L ammonium acetate solution（1∶1）by isocratic elution at a rate of 0.3 mL/min.Then the samples were ionized using positive electrospray ionization（ESI＋）,examined by multiple reaction monitoring（MRM）mode and quantitated by external standard method.An excellent linear relationship was obtained within the range of 0.6-30.0 ng for four aflatoxins with correlation coefficients of 0.99904-0.99999.Average recoveries obtained from spiked sample at three concentration levels were between 73.8%and 100.8%.The method is rapid,sensitive,accurate and specific for the determination and comfirmation of four kinds of aflatoxins in traditional Chinese medicines.
作者
朱筱玲
ZHU Xiao-ling(Jiangxi Province Institute of Analysis and Testing,Nanchang 33002)
出处
《分析科学学报》
CAS
CSCD
北大核心
2018年第5期673-676,共4页
Journal of Analytical Science
