高效液相色谱-串联质谱法测定葡萄酒中纳他霉素的含量  

HPLC-MS/MS Determination of Natamycin in Grape Wine

作　　者：崔淑华[1] 程刚[1] 张雪琰[1] 李正义[1] 王宇[1] 赵峰[1] 

机构地区：[1]山东出入境检验检疫局检验检疫技术中心,青岛266002

出　　处：《理化检验（化学分册）》2016年第9期1036-1040,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家质量监督检验检疫总局出入境检验检疫行业标准制订计划(2014B199K)

摘　　要：取葡萄酒样品5.00mL于棕色容量瓶中,用乙腈-0.1%(φ)甲酸溶液(5+95)的混合液稀释至50mL,离心5min使小粒径杂质下沉后,取上清液进行液相色谱分离。用Eclipse plus C18色谱柱作为固定相,用不同比例的乙腈和0.1%甲酸溶液的混合液作流动相进行梯度淋洗。质谱分析中采用电喷雾离子源正离子扫描、多反应监测模式。制作标准曲线时,须用与样品相同类型的空白葡萄酒作为稀释剂,以消除样品的基质效应。纳他霉素的质量浓度在0.20~100μg·L^(-1)范围内与其相应峰面积值呈线性关系。红、白、桃红葡萄酒的检出限(3S/N)分别为0.099,0.024,0.046μg·L^(-1)。按标准加入法在3个浓度水平上进行加标回收试验,测得回收率在87.0%~102%之间,测定值的相对标准偏差(n=5)在4.0%~7.7%之间。Sample of grape wine （5. 00 mL） was diluted with a mixture of acetonitrile-0. 1% （φ） formic acid （5＋95） to 50 mL in a brown glass volumetric flask, and a portion of the solution was centrifuged for 5 min to have the small grained impurities settled. The supernatant was used for LC separation. Eclipse plus C18 column was used as stationary phase and mixtures of acetonitrile and 0. 1% （φ） formic acid in various ratios were used as mobile phase in gradient elution. In MS/MS analysis, ESI＋ scanning and MRM were adopted. In preparation of standard curves, blank wine sample of same variety with the objective sample used as the matrix solution to dilute standard solution of natamycin, in order to match the matrix effect. Linear relationship between values of peak area and mass concentration of natamycin was obtained in the range of 0. 20-100 μg·L^-1 , and values of detection limits （3S/N） found for red, white and rose wine were 0. 099, 0. 024, 0. 046 μg·L^-1 respectively. Tests for recovery were made by standard addition method at 3 concentration levels, giving results in the range of 87.0%- 102%, with RSDs （n=5） ranged from 4. 0% to 7.7%.

关 键 词：高效液相色谱-串联质谱法 纳他霉素 葡萄酒 

分 类 号：O657.63[理学—分析化学]