摘要
依次采用磷酸盐缓冲液(PBS)和甲醇-PBS溶液提取样品,以多功能免疫亲和柱净化,采用液相色谱-串联四极杆质谱检测,可同时测定中药材中的黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、伏马毒素B1、伏马毒素B2、T-2毒素、HT-2毒素、赭曲霉毒素A(OTA)、玉米赤霉烯酮等14种真菌毒素。优化条件下,真菌毒素的定量限(LOQ)为1～5μg/kg,4种中药材基质(人参、桔梗、板蓝根、麦门冬)中3个不同添加水平的平均回收率(n=6)为71.9%～99.7%,相对标准偏差(RSD)为4.8%～15.8%。该方法的检测速度快,中药材复杂基质的干扰较少,结果准确、可靠,定量限可满足国内外中药材真菌毒素相关限量的要求。
A method was developed for the determination of 14 mycotoxins,aflatoxins,T-2, HT-2,fumonisins,ochratoxin A,zearalenone,etc.in Chinese herbs by liquid chromatography-tandem quadrupole mass spectrometry（LC-MS/MS）.The sample was extracted with phosphate buffer solution（PBS） and methanol in turn,and then purified by a high selective multifunctional immunoaffinity column.The column was washed by PBS（containing 0.1% Twain） and water,and then eluted by methanol.The eluate was dried under nitrogen,dissolved in methanol-10 mmol/L NH4Ac（40∶60,v/v） solution.The mycotoxins were separated on a Waters Xterra C18 MS column（100 mm×2.1 mm,3.5 μm） and detected by MS/MS.The limits of quantification（LOQs） of the 14 mycotoxins were from 1.0 to 5.0 μg/kg.The average recoveries of the 14 mycotoxins spiked in Chinese herbs（Ginseng,Campanulaceae,Radix and Ophiopogonis） ranged from 71.9% to 99.7% at the three spiked levels of 1.0,5.0,10.0 μg/kg,and the relative standard deviations（RSDs,n=6） were between 4.8% and 15.8%.The method is rapid,sensitive and accurate,and suitable for the determination of the 14 mycotoxins in Chinese medicines.The quantification limits of aflatoxins can meet the domestic and foreign requirements.
出处
《色谱》
CAS
CSCD
北大核心
2011年第6期495-500,共6页
Chinese Journal of Chromatography
基金
国家质量监督检验检疫总局科研课题资助项目(2008IK144)
关键词
免疫亲和柱净化
液相色谱-串联质谱
真菌毒素
中药材
immunoaffinity column purification
liquid chromatography-tandem mass spectrometry（LC-MS/MS）
mycotoxins
Chinese herbs
