白酒中三氯蔗糖的HPLC及UPLC-MS/MS检测对比研究

Comparison of HPLC and UPLC-MS/MS for Determination of Sucralose in Chinese Spirit

目的 采用高效液相色谱法(HPLC)和超高效液相色谱-串联质谱法(UPLC-MS/MS)测定白酒中的三氯蔗糖,并对两种方法进行比较。方法 HPLC采用Waters Symmetry Shield C_(18)(4.6 mm×250 mm,5μm)色谱柱,示差检测器,以乙腈-水=15:85(v/v)为流动相进行等度洗脱。UPLC-MS/MS采用ACQUITY UPLC BEH C_(18)(2.1 mm×100 mm,1.7μm)色谱柱,以甲醇-0.1%甲酸水溶液为流动相,梯度洗脱,在电喷雾离子源(ESI)负离子模式下,采用多反应监测(MRM)模式进行测定。结果 HPLC线性方程为:Y=170 193.25X+697.5,相关系数(R^(2))为0.9997,检出限为2.5 mg/kg,定量限为7.50 mg/kg,回收率为85.40%~97.80%,RSD为2.98%~8.27%。UPLC-MS/MS线性方程为:Y=16.9X-59.1,R^(2)=0.9993,检出限为0.02 mg/kg,定量限为0.06 mg/kg,回收率为96.50%~98.70%,RSD为1.25%~5.73%。结论 UPLC-MS/MS灵敏度较高、选择性较好,操作更加简便,能满足白酒中三氯蔗糖残留的检测要求。

Objective To establish a method for the determination of sucralose in Chinese spirit by high performance liquid chromatography (HPLC) and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),and to evaluate the feasibility of the two methods.Methods HPLC was performed on a Waters Symmetry Shield C_(18)(4.6 mm×250 mm,5μm) column equipped with refractive index detector,using CH_(3)CN-H_(2)O=15:85 (v/v) as the mobile phase of isocratic elution.UPLC-MS/MS was performed on an ACQUITY UPLC BEH C_(18) column(2.1 mm×100 mm,1.7μm),using methanol-0.1%aqueous formic acid as the mobile phase of gradient elution.Under the negative ion mode of electrospray ion source (ESI),multiple reaction monitoring (MRM) mode was adopted for determination.Results The linear equation of HPLC was Y=170 193.25X+697.5,with correlation coefficient (R^(2)) of0.9997;the limit of detection (LOD) was 2.5 mg/kg,and the limit of quantitation (LOQ) was 7.5 mg/kg;the recoveries were 85.40%-97.80%,with RSDs of 2.98%-8.27%.The linear equation of UPLC-MS/MS was Y=16.9X-59.1,with correlation coefficients (R^(2)) of 0.9993;the LOD and LOQ were 0.02 mg/kg and 0.06 mg/kg,respectively;the recoveries were 96.50%-98.70%,with RSDs of 1.25%-5.73%.Conclusion UPLC-MS/MS has advantages of higher sensitivity,better selectivity and more simple operation,which can meet the requirements for the determination of sucralose residues in Chinese spirit.