高效液相色谱-线性离子阱串联质谱技术用于白酒中甜蜜素测定的确证分析

Determination of sodium cyclamate in liquor by high performance liquid chromatography-tandem mass spectrometry with linear trap technology

建立了白酒中甜蜜素的高效液相色谱-线性离子阱串联质谱测定方法。该方法可同时准确定性和定量。样品无需前处理,过膜后直接进样,由C18色谱柱分离,采用多反应监测(MRM)和触发增强子离子扫描模式检测,采集到的MRM数据用于定量测定,同时得到的高质量子离子谱图用于谱图库检索的方法进行定性确证分析。本文采用外标法定量,方法的线性范围为1.320～132.0μg/L(r=0.999 1);检出限(信噪比为3)为0.1μg/L;添加水平分别为2.640、26.40、100.0μg/L的3个样品的加标回收率为96.38%～107.2%,相对标准偏差均小于9%;阳性样品的谱图匹配度均高于92%。该方法简便、准确、高效,适用于白酒中甜蜜素的测定及阳性样品的确证分析。

An accurate determination of quantitative and confirmative method for sodium cycla- mate in liquor by high performance liquid chromatography-tandem mass spectrometry （HPLC- MS/MS） with linear trap technology has been established. Without pretreatment, the sample was directly injected after filtering through a 0.2 μm micro filter. The HPLC separation was performed on an Atlantis dC18 column （ 150 mm× 2. 1 mm, 3μm） by gradient elution with methanol and water containing 0. 1% （v/v） formic acid. The eluent was determined and con-firmed in multiple reaction monitoring-enhanced product ion （MRM-EPI） scan mode. The acquired data from MRM for the quantitative determination, and the product ion spectra were used for library search for qualitative confirmatory analysis. External standard was used for the quantitative determination of sodium cyclamate in liquor, and good linearity （ r = 0. 9991 ） was obtained over the range of 1. 320 - 132.0 μg/L. The limit of detection （ LOD, S/N=3 ） for sodium cyclamate was 0. 1μg/L. The average recoveries ranged from 96.38% to 107.2% at thespiked levels of 2. 640, 26.40 and 100.0μg/L with the relative standard deviations （RSDs） less than 9%. The matching degrees of the spectra for all positive samples were higher than 92%. The method is simple, accurate and efficient for the determination of sodium cyclamate in liquor and particularly suitable for confirmatory analysis of positive samples.