摘要
目的建立胶类中药产品中的4种黄曲霉毒素残留量的免疫亲和柱净化-高效液相色谱-串联四级杆质谱(HPLC-MS/MS)检测方法。方法以体积分数60%甲醇为溶剂提取,X-Brigde-C_(18)(3.0 mm×50 mm,3.5μm)色谱柱分离,串联四级杆质谱仪检测,MRM模式进行定性定量分析检测阿胶、鹿角胶以及龟甲胶中的黄曲霉毒素B_1、B_2、G_1、G_2。结果 4种黄曲霉毒素质谱检测的线性范围宽,相关性好,r≥0.997 9;方法精密度以6次测定值的RSD表示,为1.2%~4.1%;方法回收率用3个浓度进行添加实验,回收率范围为77.3%~94.6%;定量限范围为0.5~0.8μg·L^(-1);日内精密度RSD(n=5)范围为1.1%~2.9%,日间精密度RSD(n=9)范围为1.5%~2.8%。结论本方法专属性强,操作简单,快捷,可作为阿胶、鹿角胶以及龟甲胶中黄曲霉毒素定量定性的有效检测方法。
OBJECTIVE To develop an immunoaffinity column clean-up and high iaerformance liquid chromatography coupled with triple quadrupole mass spectrometry（HPLC-MS/MS） method to determine aflatoxins in gelatin drags. METHODS The analysis was performed by an HPLC-MS/MS system with X-Brigde-C18 （ 3.0 mmx 50 mm, 3.5 μm） column. Multiple-reaction monitoring （MRM） was performed to identify and quantify aflatoxin B1 , B2, G1 and G2 , which were extracted from Asini Coril Colla, Cervil Comus Colla, and Testudinis Carapacis Colla with 60% methanol solution. RESULTS Linear calibration curves were obtained with r〉 0. 997 9. The precision of the method was showed by RSDs （n =6） ranging from 1.2% to 4. 1%. The recoveries were determined at three concentration levels and ranged from 77.3% to 94. 6%. The ranges of LOQs were from 0. 5 to 0. 8 μg· L-1 and the RSDs （n = 9 ） of intra-day precision and inter-day precision were from 1.1% to 2. 9% and from 1.5% to 2. 8% , respectively. CONCLUSION The method is specific, simple and rapid to detect aflatoxins in gelatin drags.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2017年第17期1542-1546,共5页
Chinese Pharmaceutical Journal
