Simultaneous Determination of Sweeteners and Pigments in Essences and Spices by UHPLC-MS/MS
摘 要
采用超高效液相色谱-串联质谱法同时测定香精、香料中的3种甜味剂和5种色素。样品经氨水-甲醇混合溶液提取后,采用Waters BEH C18色谱柱分离,以不同比例的10 mmol·L-1乙酸铵溶液(此溶液每升含冰乙酸1 mL)和甲醇的混合液为流动相进行梯度洗脱。对甜味剂采用电喷雾负离子模式,对色素采用电喷雾正离子模式,采用多反应监测模式进行测定。8种待测物质的质量浓度在一定范围内与峰面积呈线性关系,检出限(3S/N)在0.09~1.2 mg·kg-1之间。加标回收率在82.9%~118%之间,测定值的相对标准偏差(n=5)均小于6%。
Abstract
UHPLC-MS/MS was applied to the determination of 3 sweeteners and 5 pigments in samples of essence or spice. The sample was extracted with a mixture of methanol and ammonia. The extract was separated on Waters BEH C18 column, with a mixture of methanol and 10 mmol·L-1 ammonium acetate solution (containing 1 mL of glacial acetic acid per liter of solution) in various ratios as mobile phase in gradient elution. ESI+ (for pigment sample), ESI- (for sweetener sample) and MRM were adopted in MS. Linear relationships were found between values of peak areas and mass concentrations of the 8 analytes in definite ranges, with detection limits (3S/N) in the range of 0.09-1.2 mg·kg-1. Results of test for recovery found by standard addition method were in the range of 82.9%-118%, and RSD′s (n=5) were less than 6%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201512021
所属栏目 工作简报
基金项目 云南中烟公司科研资助项目(2013CP03;2015JC04)
收稿日期 2014/11/20
修改稿日期
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备注李晶(1982-),女,云南大理人,工程师,博士,主要 从事色谱、质谱分析研究。
引用该论文: LI Jing,YANG Ye-kun,CHEN Jian-hua,MIAO En-ming,GENG Yong-qin,DUAN Kai,LI Xue-mei,XU Ji-cang. Simultaneous Determination of Sweeteners and Pigments in Essences and Spices by UHPLC-MS/MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(12): 1724~1728
李晶,杨叶昆,陈建华,缪恩铭,耿永勤,端凯,李雪梅,徐济仓. 超高效液相色谱-串联质谱法测定香精香料中的甜味剂和色素[J]. 理化检验-化学分册, 2015, 51(12): 1724~1728
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参考文献
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【7】ARMENTA S, GARRIGUES S, GUARDIA M. Sweeteners determination in table top formulations using FT-Raman spectrometry and chemometric analysis[J]. Anal Chim Acta, 2004,521(2):149-155.
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【13】黄永辉,余清,林钦,等.超高效液相色谱法同时测定碳酸饮料中的22种食品添加剂[J].分析测试学报, 2011,30(8):877-882.
【14】肖立群,张承聪,张承明.超高效液相色谱法测定食品中5种人工合成甜味剂[J].理化检验-化学分册, 2012,48(12):1427-1429.
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【16】李帮悦,冯家力,潘振球,等.高效液相色谱-质谱/质谱联用法测定饮料中的人工合成色素[J].中国卫生检验杂志, 2007,17(4):579-585.
【17】FERRER I, THURMAN E M. Analysis of sucralose and other sweeteners in water and beverage samples by liquid chromatography/time-of-flight mass spectrometry[J]. J Chromatogr A, 2010,1217(25):4127-4134.
【18】赵延胜,杨敏莉,张峰,等.液相色谱/四极杆-飞行时间质谱法筛查奶酪中29种禁用和限用合成色素[J].色谱, 2011,29(7):631-636.
【19】嵇超,冯峰,陈正行,等.高效液相色谱-串联质谱法测定葡萄酒中的5种人工合成甜味剂[J].色谱, 2010,28(8):749-753.
【20】刘晓霞,丁利,刘锦霞,等.高效液相色谱-串联质谱法测定食品中6种人工合成甜味剂[J].色谱, 2010,28(11):1020-1025.
【21】李晶,徐济仓,李雪梅,等.超高效液相色谱法同时测定香精香料中14种禁限用物质[J].色谱, 2012,30(8):816-821.
【22】STORM T, REEMTSMA T, JEKEL M. Use of volatile amines as ion-pairing agents for the high performance liquid chromatographic-tandem mass spectrometric determination of aromatic sulfonates in industrial wastewater[J]. J Chromatogr A, 1999,854(1/2):175-185.
【23】冯峰,杨烁,凌云,等.超高效液相色谱-串联质谱快速筛查葡萄酒中的14种禁用食品添加剂[J].分析化学, 2011,39(11):1732-1737.
【2】GB/T 2760-2011 食品添加剂使用标准[S].
【3】GB/T 23495-2009 食品中苯甲酸、山梨酸和糖精钠的测定 高效液相色谱法[S].
【4】GB/T 5009.140-2003 饮料中乙酰磺胺酸钾的测定[S].
【5】GB/T 5009.35-2003 食品中合成着色剂的测定[S].
【6】CABERO C, SAURINA J, HERNNDEA-CASSOU S. Flow-injection spectrophotometric determination of cyclamate in sweetener products with sodium 1,2-naphthoquinone-4-sulfonate[J]. Anal Chim Acta, 1999,381(2/3):307-313.
【7】ARMENTA S, GARRIGUES S, GUARDIA M. Sweeteners determination in table top formulations using FT-Raman spectrometry and chemometric analysis[J]. Anal Chim Acta, 2004,521(2):149-155.
【8】PESEK J J, MATYSKA M T. Determination of aspartame by high-performance capillary electrophoresis[J]. J Chromatogr A, 1997,781(1/2):423-428.
【9】FRAZIER R A, INNS E L, DOSSI N, et al. Development of a capillary electrophoresis method for the simultaneous analysis of artificial sweeteners, preservatives and colours in soft drinks[J]. J Chromatogr A, 2000,876(1/2):213-220.
【10】CHEN Qing-chuan, WANG Jing. Simultaneous determination of artificial sweeteners, preservatives, caffeine, theobromine and theophylline in food and pharmaceutical preparations by ion chromatography[J]. J Chromatogr A, 2002,937(1/2):57-64.
【11】ZHU Y, GUO Y, YE M, et al. Separation and simultaneous determination of four artificial sweeteners in food and beverages by ion chromatography[J]. J Chromatogr A, 2005,1085(1):143-146.
【12】WASIK A, MCCOURT J, BUCHGRABER M. Simultaneous determination of nine intense sweeteners in foodstuffs by high performance liquid chromatography and evaporative light scattering detection-development and single-laboratory validation[J]. J Chromatogr A, 2007,1157(1/2):187-196.
【13】黄永辉,余清,林钦,等.超高效液相色谱法同时测定碳酸饮料中的22种食品添加剂[J].分析测试学报, 2011,30(8):877-882.
【14】肖立群,张承聪,张承明.超高效液相色谱法测定食品中5种人工合成甜味剂[J].理化检验-化学分册, 2012,48(12):1427-1429.
【15】盛旋,陈昌骏,丁振华,等.固相萃取-液相色谱/质谱法同时测定食品中磺胺类人工合成甜味剂[J].分析试验室, 2006,25(7):75-78.
【16】李帮悦,冯家力,潘振球,等.高效液相色谱-质谱/质谱联用法测定饮料中的人工合成色素[J].中国卫生检验杂志, 2007,17(4):579-585.
【17】FERRER I, THURMAN E M. Analysis of sucralose and other sweeteners in water and beverage samples by liquid chromatography/time-of-flight mass spectrometry[J]. J Chromatogr A, 2010,1217(25):4127-4134.
【18】赵延胜,杨敏莉,张峰,等.液相色谱/四极杆-飞行时间质谱法筛查奶酪中29种禁用和限用合成色素[J].色谱, 2011,29(7):631-636.
【19】嵇超,冯峰,陈正行,等.高效液相色谱-串联质谱法测定葡萄酒中的5种人工合成甜味剂[J].色谱, 2010,28(8):749-753.
【20】刘晓霞,丁利,刘锦霞,等.高效液相色谱-串联质谱法测定食品中6种人工合成甜味剂[J].色谱, 2010,28(11):1020-1025.
【21】李晶,徐济仓,李雪梅,等.超高效液相色谱法同时测定香精香料中14种禁限用物质[J].色谱, 2012,30(8):816-821.
【22】STORM T, REEMTSMA T, JEKEL M. Use of volatile amines as ion-pairing agents for the high performance liquid chromatographic-tandem mass spectrometric determination of aromatic sulfonates in industrial wastewater[J]. J Chromatogr A, 1999,854(1/2):175-185.
【23】冯峰,杨烁,凌云,等.超高效液相色谱-串联质谱快速筛查葡萄酒中的14种禁用食品添加剂[J].分析化学, 2011,39(11):1732-1737.
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