高效液相色谱-串联质谱法同时测定葡萄酒中甜味剂、防腐剂和色素
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摘要
建立了高效液相色谱-串联质谱仪(HPLC-MS/MS)同时测定葡萄酒中甜味剂(安赛蜜、糖精钠、甜蜜素、阿斯巴甜、三氯蔗糖、纽甜、阿力甜和甜菊糖苷)、防腐剂(脱氢乙酸)和色素(诱惑红、赤藓红、苋菜红、胭脂红、柠檬黄、日落黄、亮蓝)含量的新方法。样品经超纯水稀释5倍,微孔滤膜过滤后直接进样,用HPLC-MS/MS进行定量分析。Acquity UPLC HSS T_3柱为分析柱,甲醇-10 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,采用电喷雾离子源(ESI)正负离子切换多反应监测模式(MRM)检测,外标法定量。结果表明,16种添加剂在相应的浓度范围内线性关系良好(相关系数r~2>0.995),方法检出限在0.2～3μg/L之间,在3个不同浓度的添加水平下,平均回收率为89.1%～106.4%,相对标准偏差≤9.7%,满足日常检测的要求。该方法前处理简单,测定快速、准确、灵敏度高,适用于葡萄酒中16种添加剂的快速筛查和定量分析。
A method for simultaneous determination of sweeteners(acesulfame potassium,sodium saccharin,sodium cyclamate,aspartame,sucralose,neotame,alitame and stevioside),preservatives(dehydroacetic acid),and pigments(allura red,erythrosine,amaranth,carmine,lemon yellow,sunset yellow,brilliant blue) had been developed.Wine samples were diluted with distilled water(five times of wine volume),then filtered through 0.22 μm microporous membrane,and quantitative analysis was done by HPLC-MS/MS through direct sample injection.LC separation was performed on Shimadzu LC-20 ADXR system with a T_3 column,acetic acid ammonium(10 mmol/L) and methanol was used as the mobile phase for gradient elution.After LC separation,MS/MS was adopted for multiple reaction monitoring(MRM) in the positive and negative mode.The correlation coefficients of linear calibration curves were higher than 0.995 in the corresponding concentration ranges.The limits of detection(LODs) were between 0.2 μg/L to 3 μg/L.The average recoveries of the 16 additives ranged from 89.1 % to 106.4 %,and the relative standard deviations(RSD) were lower than9.7 % in spiked sample at three levels.The results indicated that this method was easier,faster,more sensitive,and suitable for qualitative and quantitative analysis of preservatives,sweeteners and pigments in wine.
A method for simultaneous determination of sweeteners(acesulfame potassium,sodium saccharin,sodium cyclamate,aspartame,sucralose,neotame,alitame and stevioside),preservatives(dehydroacetic acid),and pigments(allura red,erythrosine,amaranth,carmine,lemon yellow,sunset yellow,brilliant blue) had been developed.Wine samples were diluted with distilled water(five times of wine volume),then filtered through 0.22 μm microporous membrane,and quantitative analysis was done by HPLC-MS/MS through direct sample injection.LC separation was performed on Shimadzu LC-20 ADXR system with a T_3 column,acetic acid ammonium(10 mmol/L) and methanol was used as the mobile phase for gradient elution.After LC separation,MS/MS was adopted for multiple reaction monitoring(MRM) in the positive and negative mode.The correlation coefficients of linear calibration curves were higher than 0.995 in the corresponding concentration ranges.The limits of detection(LODs) were between 0.2 μg/L to 3 μg/L.The average recoveries of the 16 additives ranged from 89.1 % to 106.4 %,and the relative standard deviations(RSD) were lower than9.7 % in spiked sample at three levels.The results indicated that this method was easier,faster,more sensitive,and suitable for qualitative and quantitative analysis of preservatives,sweeteners and pigments in wine.
引文
[1]李晶,徐济仓,谬明明,等.固相萃取-超高效液相色谱/串联质同时检测饮料中13种禁限用食品添加剂[J].分析测试学报, 2013, 29(4):488-492.
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[12]牟霄,张璐,张崇淼,等.超高效液相色谱法同时测定饮料中14种食品添加剂[J].食品安全质量检测学报,2017(8):3177-3184.
[13]杨仁君,孙洁,李好转,等.离子色谱法同时测定白酒中3种甜味剂方法探讨[J].酿酒科技,2016(9):122-124.
[14] KOKYA T A, FARHADI K, KALHORI A A M.Optimized dispersive liquid-liquid microextraction and determination of sorbic acid and benzoic acid in beverage samples by gas chromatography[J]. Food analytical methods, 2012, 5(3):351-358.
[15] LIU T, JIANG Z T, LI R, et al. Simultaneous determination of cyclamate, acesulfame, and aspartame in beverages by titania-based RP-HPLC[J]. Food analytical methods, 2014, 7(7):1400-1406.
[16] GREMBECKA M, BARAN P, B?A?EWICZ A, et al.Simultaneous determination of aspartame, acesulfameK, saccharin, citric acid and sodium benzoate in various food products using HPLC-CAD-UV/DAD[J]. Eur food res technol,2014,238:357-365.
[17] KUBICA P, NAMIE?NIK J, WASIK A. Determination of eight artificial sweeteners and common Stevia rebaudiana glycosides in non-alcoholic and alcoholic beverages by reversed-phase liquid chromatography coupled with tandem mass spectrometry[J]. Anal bioanal chem, 2015,407:1505-1512.
[18] ZYGLER A, WASIK A, KOT-WASIK A, et al.Determination of nine high-intensity sweeteners in various foods by high-performance liquid chromatography with mass spectrometric detection[J].Anal bioanal chem,2011,400:2159-2172.
[19]伊雄海,邓晓军,杨惠琴,等.液相色谱-串联质谱法检测食品中的多种易滥用着色剂[J].色谱, 2011, 29(11):1062-1069.
[20] LIM H S, PARK S K, KWAK I S, et al. HPLC-MS/MS analysis of 9 artificial sweeteners in imported foods[J].Food sci biotechnol, 2013,22(S):233-240.
[21]牛之瑞,王秀君,于毅涛,等.液相色谱-质谱联用同时测定白酒中8种甜味剂[J].食品科学, 2016, 37(2):178-181.
[22]王萍亚,周勇,戴意飞,等.超高效液相色谱:四极杆飞行时间质谱法快速筛查水产品中28种酸性合成色素[J].色谱, 2015, 33(8):822-829.
[23]罗辉泰,黄晓兰,吴惠勤,等.分散固相萃取-同位素稀释-高效液相色谱-串联质谱法同时测定猪肉中26种-β受体激动剂[J].色谱, 2016, 34(5):481-489.
[24]宋卫得,袁晓鹰,吕宁,等.梯度淋洗-电导抑制离子色谱色谱法同时测定果汁中26种有机酸和阴离子[J].色谱, 2016, 34(11):1084-1090.
[2]赵飞,高广慧,那海秋,等.固相萃取-高效液相色谱-可变波长检测法同时测定调味品中甜味剂和人工合成色素[J].色谱, 2013, 31(5):490-493.
[3] MA K, LI X J, WANG H F, et al. Rapid and sensitive method for the determination of eight food additives in red wine by ultra-performance liquid chromatography tandem mass spectrometry[J].Food anal,2015,8:203-212.
[4]陈晓红,赵永纲,姚珊珊,等.超快速液相色谱-串联质谱法测定黄酒和葡萄酒中的9种防腐剂和甜味剂[J].色谱, 2011, 29(12):1147-1154.
[5]龙飞,丁怡.葡萄酒中11种添加剂的快速检测.酿酒科技[J]. 2014(3):97-100.
[6]吕梦莎,林能镖,梁玉英.高效液相色谱法同时测定葡萄酒中16种添加剂[J].食品科学, 2016, 37(8):222-225.
[7]黎永乐,郑彦婕,熊岑,等.液相色谱/线性离子阱-静电场轨道阱高分辨质谱法快速筛查葡萄酒中的合成色素[J].色谱, 2013,31(8):729-733.
[8]高莹,高杰,张勋,等.基于液相色谱-串联质谱法检测多种食品中的9种非食用色素[J].食品与发酵工业,2016, 42(1):183-188.
[9]国家卫生和计划生育委员会.食品安全国家标准食品中苯甲酸、山梨酸和糖精钠的测定:GB 5009.28—2016[S].北京:中国标准出版社,2017.
[10]国家卫生和计划生育委员会.食品安全国家标准食品中阿斯巴甜和阿力甜的测定:GB 5009.263—2016[S].北京:中国标准出版社,2017.
[11]国家卫生和计划生育委员会.食品安全国家标准食品中合成着色剂的测定:GB 5009.35—2016[S].北京:中国标准出版社,2017.
[12]牟霄,张璐,张崇淼,等.超高效液相色谱法同时测定饮料中14种食品添加剂[J].食品安全质量检测学报,2017(8):3177-3184.
[13]杨仁君,孙洁,李好转,等.离子色谱法同时测定白酒中3种甜味剂方法探讨[J].酿酒科技,2016(9):122-124.
[14] KOKYA T A, FARHADI K, KALHORI A A M.Optimized dispersive liquid-liquid microextraction and determination of sorbic acid and benzoic acid in beverage samples by gas chromatography[J]. Food analytical methods, 2012, 5(3):351-358.
[15] LIU T, JIANG Z T, LI R, et al. Simultaneous determination of cyclamate, acesulfame, and aspartame in beverages by titania-based RP-HPLC[J]. Food analytical methods, 2014, 7(7):1400-1406.
[16] GREMBECKA M, BARAN P, B?A?EWICZ A, et al.Simultaneous determination of aspartame, acesulfameK, saccharin, citric acid and sodium benzoate in various food products using HPLC-CAD-UV/DAD[J]. Eur food res technol,2014,238:357-365.
[17] KUBICA P, NAMIE?NIK J, WASIK A. Determination of eight artificial sweeteners and common Stevia rebaudiana glycosides in non-alcoholic and alcoholic beverages by reversed-phase liquid chromatography coupled with tandem mass spectrometry[J]. Anal bioanal chem, 2015,407:1505-1512.
[18] ZYGLER A, WASIK A, KOT-WASIK A, et al.Determination of nine high-intensity sweeteners in various foods by high-performance liquid chromatography with mass spectrometric detection[J].Anal bioanal chem,2011,400:2159-2172.
[19]伊雄海,邓晓军,杨惠琴,等.液相色谱-串联质谱法检测食品中的多种易滥用着色剂[J].色谱, 2011, 29(11):1062-1069.
[20] LIM H S, PARK S K, KWAK I S, et al. HPLC-MS/MS analysis of 9 artificial sweeteners in imported foods[J].Food sci biotechnol, 2013,22(S):233-240.
[21]牛之瑞,王秀君,于毅涛,等.液相色谱-质谱联用同时测定白酒中8种甜味剂[J].食品科学, 2016, 37(2):178-181.
[22]王萍亚,周勇,戴意飞,等.超高效液相色谱:四极杆飞行时间质谱法快速筛查水产品中28种酸性合成色素[J].色谱, 2015, 33(8):822-829.
[23]罗辉泰,黄晓兰,吴惠勤,等.分散固相萃取-同位素稀释-高效液相色谱-串联质谱法同时测定猪肉中26种-β受体激动剂[J].色谱, 2016, 34(5):481-489.
[24]宋卫得,袁晓鹰,吕宁,等.梯度淋洗-电导抑制离子色谱色谱法同时测定果汁中26种有机酸和阴离子[J].色谱, 2016, 34(11):1084-1090.