建立了超高效液相色谱-串联三重四极杆质谱(ultra-performance liquid chromatography-mass spectrometry/mass spectrometry, UPLC-MS/MS)快速筛查和确证饮料中茶碱、咖啡因2种生物碱和糖精钠、安赛蜜、阿斯巴甜、纽甜、爱德万甜、三氯蔗糖6种甜味剂的方法。样品经乙腈-水(20∶80,V/V) 超声提取,离心,过滤,经超高效液相色谱分离后,在电喷雾离子源的正负离子电离模式下,用多反应监测(multiple reaction monitoring, MRM) 方式采集数据,根据保留时间和定性离子对进行定性筛查,根据峰面积和定量离子对进行定量分析。2种生物碱和6种甜味剂的方法检出限(limit of detection, LOD)为0.003~0.5 mg/kg (信噪比S/N≥3),定量限(limit of quantity, LOQ)为0.01~2 mg/kg(S/ N≥10),回收率为92.3%～110.4%,RSD为0.9%～10.8%。在0.001～14.088 μg/mL均有良好的线性,相关系数r均大于0.995。该方法快速、简便、准确、灵敏度高,适用于饮料中2种生物碱和6种甜味剂的批量检测。
A new ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with triple quadrupole method was developed in order to determine theophylline, caffeine, saccharin, acesulfame, aspartame, neotame, advantame and sucralose in beverages. Samples were ultrasonically extracted with acetonitrile and water (20∶80, v/v), followed by centrifugation and filtration. The target compound was separated by UPLC, and positive and negative electrospray ionization at multiple reaction monitoring (MRM) mode was applied. Qualitative screening was achieved with retention time and qualitative ions, and peak area and quantitative ions were used for quantification. The results showed that the limit of detection of the method was 0.003-0.5 mg/kg and the limit of quantification was 0.01-2 mg/kg. The average recovery showed a variation from 92.3% to 110.4% and the RSD was 0.9%-10.8%. Besides, a good linear relationship was found in the range of 0.001-14.088 μg/mL target compounds with correlation coefficients being above 0.995. Overall, this method was rapid, simple, sensitive and accurate, which is suitable for batch determination of the 2 alkaloids and 6 sweetening agents in beverages.
[1] 王翔,李萍艳,万再聪,等. 绿茶中提取咖啡因的方法研究[J]. 安徽农业科学,2009,37(8):3 598-3 599.
[2] 张倩勉,盘正华,范兴,等.HPLC-MS法测定饮料中甜蜜素等6种非糖类甜味剂含量[J].安徽农业科学,2017,45(13):99-102;118.
[3] 国家卫生计生委.中华人民共和国国家卫生和计划生育委员会第 8号公告[EB/OL]. (2017-10-20) .http://www.nhfpc.gov.cn/sps/s7890/201710/c4cc46c01005 445f88ad169c8e 820aee.Shtml
[4] GB 5009.28－2016食品安全国家标准食品中苯甲酸.山梨酸和糖精钠的测定[S].北京:中国标准出版社,2016.
[5] GBT 5009.140－2003饮料中乙酰磺胺酸钾的测定[S].北京:中国标准出版社,2012.
[6] GB 5009.263－2016食品安全国家标准食品中阿斯巴甜和阿力甜的测定[S].北京:中国标准出版社,2016.
[7] GB 5009.247－2016食品安全国家标准食品中纽甜的测定[S].北京:中国标准出版社,2016.
[8] GB5009.139－2014食品安全国家标准食品中咖啡因的测定[S].北京:中国标准出版社,2014.
[9] GB 22255－2014食品安全国家标准食品中三氯蔗糖(蔗糖素)的测定[S].北京:中国标准出版社,2014.
[10] 汪辉,黄小贝,刘江,等.超高效液相色谱-串联质谱快速测定食品中的新品种甜味剂爱德万甜[J].色谱,2018,36(7):700-704.
[11] 汪辉,曹阳,曹雄杰,等.高效液相色谱法测定食品中的爱德万甜[J].分析测试学报,2018,37(5):635-638.
[12] 曾永芳,覃昆飞,李莜.超高效液相色谱法同时测定奶茶饮品中的10种添加剂[J].中国卫生检验杂志,2018,28(15):1 806-1 809;1 813.
[13] 郑佳,郗存显,曹淑瑞,等.QuEChERS-超高效液相色谱-串联质谱法同时测定保健食品中21种非法添加化学药物[J].色谱,2017,35(12):1 257-1 265.
[14] TSO J,AGA D S.A systematic investigation to optimize simultaneous extraction and liquid chromatography tandem mass spectrometry analysis of estrogens and their conjugated metabolites in milk [J]. J Chromatogr A,2010,1217(29): 4 784-4 795.
[15] 茹歌,王柯,陈丹丹,等.超高效液相色谱-串联质谱法同时测定化妆品中13种性激素含量[J].分析测试学报,2018,37(4):464-470.
