高效液相色谱-串联质谱法同时测定辣椒粉及辣椒油中的7种罗丹明染料

建立了辣椒粉及辣椒油中7种罗丹明染料的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。样品经正己烷或甲醇-水(体积比为1:1)溶液提取后,经固相萃取(SPE)柱净化,采用SB-C18柱分离,以乙腈和水(含体积分数为0.1%的甲酸)为流动相进行梯度洗脱,采用正离子模式质谱检测,在多反应监测(MRM)模式下进行定性定量测定。7种罗丹明类染料在0.0005～1.0 mg/L质量浓度范围内线性关系良好,相关系数(r2)均大于0.997;方法的检出限分别为0.21～51 μg/kg(辣椒粉)和0.19～25 μg/kg(辣椒油);方法的回收率为85.0%～106.0%,日内及日间相对标准偏差均小于20%。该方法简单、灵敏度高、分析时间短,适用于辣椒粉和辣椒油中7种罗丹明染料的同时测定。

Simultaneous determination of 7 rhodamine dyes in hot chili products by high performance liquid chromatography-tandem mass spectrometry

A credible method was developed for the simultaneous determination of 7 rhodamine dyes in hot chili products based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The samples were extracted with hexane or methanol-water (1:1, v/v) and then cleaned up by a solid phase extraction cartridge. The target analytes were separated on an SB-C18 column with gradient elution using acetonitrile and water (containing 0.1% (v/v) formic acid for both) as mobile phases. The identification and quantification were achieved by using ESI-MS/MS in positive ion mode and with multiple reaction monitoring (MRM). The linear ranges were from 0.0005 to 1.0 mg/L with the correlation coefficients (r2) above 0.997 for all the 7 rhodamine dyes. The limits of detection (LOD) in chili powder and chili oil were from 0.21 to 51 μg/kg and 0.19 to 25 μg/kg, respectively. The relative standard deviations of intra-day and inter-day were both less than 20%. The recoveries of the method were between 85.0% and 106%. The method is simple, rapid, highly sensitive and suitable for the simultaneous determination of 7 rhodamine dyes in foods.