GC-MS/MS检测吡咯喹啉醌二钠盐中5种N-亚硝胺含量  

Determination of 5 Kinds of N-Nitrosamines Contents in Pyrroloquinoline Quinone Disodium by GC-MS/MS

作　　者：王生秀 田佳怡 吕晓蕾 梁建森 黄萍 陈健 WANG Shengxiu;TIAN Jiayi;LÜXiaolei;LIANG Jiansen;HUANG Ping;CHEN Jian(Changhai Biological Company,Zhejiang Medicine Co.,Ltd.,Shaoxing 312300;Xinchang Pharmaceutical Factory,Zhejiang Medicine Co.,Ltd.,Shaoxing 312500)

机构地区：[1]浙江医药股份有限公司昌海生物分公司,绍兴312300 [2]浙江医药股份有限公司新昌制药厂,绍兴312500

出　　处：《食品工业》2024年第10期286-290,共5页The Food Industry

摘　　要：建立一种气相色谱-串联质谱法(GC-MS/MS)检测吡咯喹啉醌二钠盐中5种N-亚硝胺含量的方法。样品经0.1 mol/L氢氧化钠溶液涡旋溶解,使用二氯甲烷萃取,采用多重反应监测模式进行样品测定。5种N-亚硝胺在0.2~4.0 ng/mL线性范围内相关系数r均高于0.9970,线性关系良好。方法的检出限为0.005 mg/kg时,5种N-亚硝胺响应值均大于3,方法的定量限为0.01 mg/kg时,5种N-亚硝胺响应值均大于10。在0.01,0.1和0.2 mg/kg浓度水平上加标平均回收率在89.4%~107.2%之间,相对标准偏差(n=18)在1.1%~3.7%之间。该方法操作简便、准确可靠,适用于吡咯喹啉醌二钠盐中亚硝胺质量控制。Establish a method for determination of 5 kinds of N-nitrosamines Contents in Pyrroloquinoline Quinone Disodium by GC-MS/MS.The samples were vortex dissolved in 0.1 mol/L sodium hydroxide solution,extracted and layered with dichloromethane,and detected in multiplex reaction monitoring mode.The results showed that the 5 kinds of N-nitrosamines showed a good linearity in the concentration range of 0.2-4.0 ng/mL,with correlation coefficients(r)greater than 0.9970.When the detection limit of the method was 0.005 mg/kg,the response values of 5 kinds of N-nitrosamines were greater than 3;When the limit of quantification of the method was 0.01 mg/kg,the response values of 5 kinds of N-nitrosamines were greater than 10.The average recoveries were 89.4%-107.2%at the concentrations of 0.01,0.1 and 0.2 mg/kg,and the relative standard deviation(n=18)were 1.1%-3.7%.This method is simple,accurate and reliable,which is suitable for the quality control of nitrosamines in pyrroloquinoline quinone disodium.

关 键 词：气相色谱-串联质谱 吡咯喹啉醌二钠盐 亚硝胺 

分 类 号：TS207.3[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]