TurboFlow在线净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱法快速测定食品中违禁添加的罂粟壳

doi:10.3724/SP.J.1123.2017.06027

摘要/Abstract

摘要：

采用在线净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱（TF-UPLC-QTRAP MS）技术，建立了食品中吗啡、可待因、蒂巴因、罂粟碱、那可丁和原阿片碱6种罂粟壳标志物的快速确证检测方法。样品经0.10 mol/L盐酸提取、正己烷脱脂后，直接注入TF-UPLC-QTRAP MS进行分析。对影响净化的条件如TF-净化柱、流动相、洗脱溶液等条件进行了优化。确定以TurboFlow Cyclone MCX柱作为净化柱，Acquity BEH C₁₈柱为分析柱，甲醇-0.05%（体积分数）氨水溶液作为流动相，电喷雾正离子模式下多反应监测-触发增强子离子（MRM-IDA-EPI）扫描方式检测，以溶剂标准内标法定量。方法的检出限为0.05~0.5 μg/kg，定量限为0.2~2 μg/kg。平均加标回收率为81.1%~98.6%，相对标准偏差为2.9%~15.7%（n=6）。该方法灵敏、准确，适用于食品中非法添加罂粟壳的检测，已应用于实际样品的测定。

关键词: TurboFlow在线净化, 阿片生物碱, 超高效液相色谱-三重四极杆/复合线性离子阱质谱法, 食品, 罂粟壳

Abstract:

A fast confirmation method was developed for the determination of the six markers of pericarpium papaveris, morphine, codeine, narcotine, papavarine, thebaine and protopine in foods, by TurboFlow online purification-ultra performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry (TF-UPLC-QTRAP MS). The sample was extracted with 0.10 mol/L HCl. After the procedure of removal of lipid with hexane, the extraction solution was analyzed by TF-UPLC-QTRAP MS. The main factors influencing the purification efficiency including TurboFlow column, mobile phase and elution solution were optimized. The six opium alkaloids were detected by positive electrospray ionization tandem mass spectrometry in the multiple reaction monitoring-information-dependent acquisition-enhanced product ion (MRM-IDA-EPI) mode, and quantified by solvent standard internal standard method. The limits of detection were 0.05-0.5 μg/kg and the limits of quantification were 0.2-2 μg/kg for the six opium alkaloids. The recoveries were in the range of 81.1%-98.6% with the relative standard deviations ranging from 2.9% to 15.7% (n=6). The method is sensitive and accurate, and has been successfully applied to the detection of pericarpium papaveris illegally added in foods.

Key words: foods, opium alkaloids, pericarpium papaveris, TurboFlow online purification, ultra performance liquid chromatography-triple quadrupole/linear ion trap (UPLC-QTRAP MS)

中图分类号:

O658

张秀尧, 蔡欣欣, 张晓艺, 李瑞芬. TurboFlow在线净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱法快速测定食品中违禁添加的罂粟壳[J]. 色谱, 2017, 35(11): 1137-1144.

ZHANG Xiuyao, CAI Xinxin, ZHANG Xiaoyi, LI Ruifen. Fast determination of pericarpium papaveris illegally added in foods by TurboFlow online purification-ultra performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(11): 1137-1144.

参考文献

[1] Zhang T, Yu Z L, Sun C, et al. Guangzhou Chemical Industry, 2016, 44(11):13张婷, 俞祖亮, 孙册, 等. 广州化工, 2016, 44(11):13
[2] Dong N, Wang H Y. Chinese Journal of Chromatography, 2000, 18(6):554董南, 王海燕. 色谱, 2000, 18(6):554
[3] Yang Y, Tao R, Gao G. Chinese Journal of Analytical Chemistry, 1994, 22(10):1041杨元, 陶锐, 高舸. 分析化学, 1994, 22(10):1041
[4] Ministry of Health. List of Inedible Materials that may be Illegally Added in Food and Food Additives that are Easily to be Abused (Part A). (2008-12-12)[2017-08-28]. http://www.gov.cn/gzdt/2008-12/15/content_1178408.htm 卫生部. 《食品中可能违法添加的非食用物质和易滥用的食品添加剂品种名单(第一批)》. (2008-12-12)[2017-08-28]. http://www.gov.cn/gzdt/2008-12/15/content_1178408.htm
[5] China Food and Drug Administration. Notice of the Constituents of the Poppy Shell Found in Food Operated by 35 Catering Service Units. (2016-01-20)[2017-08-28]. http://www.sda.gov.cn/WS01/CL0087/142502.html国家食品药品监督管理总局. 关于35家餐饮服务单位经营的食品中检出罂粟壳成分的通告. (2016-01-20)[2017-08-28]. http://www.sda.gov.cn/WS01/CL0087/142502.html
[6] Liu Y Q, Wang H, Yang H M, et al. Food Research and Development, 2010, 31(7):130刘艳琴, 王浩, 杨红梅, 等. 食品研究与开发, 2010, 31(7):130
[7] Zhao D X, Fan G, Liu J L, et al. China Condiment, 2013, 38(7):87赵丹霞, 樊圭, 刘嘉亮, 等. 中国调味品, 2013, 38(7):87
[8] Liu M M, Zhang C Z, Li Y Z, et al. Food Research and Development, 2013, 34(1):91刘敏敏, 张朝正, 李延志, 等. 食品研究与开发, 2013, 34(1):91
[9] Zhu W X, Sun Z L, Yuan P, et al. Chinese Journal of Chromatography, 2014, 32(12):1333祝伟霞, 孙转莲, 袁萍, 等. 色谱, 2014, 32(12):1333
[10] Zhu W X, Yang J Z, Liu Y F, et al. Journal of Instrumental Analysis, 2015, 34(5):495祝伟霞, 杨冀州, 刘亚风, 等. 分析测试学报, 2015, 34(5):495
[11] DB 31/2010-2012
[12] Lin D Q, Wang T T, Wan C B, et al. Journal of Chinese Mass Spectrometry Society, 2017, 38(2):239林黛琴, 王婷婷, 万承波, 等. 质谱学报, 2017, 38(2):239
[13] Li H, He Y L, Chen X Q, et al. Food and Drug, 2014, 16(4):284李航, 贺亚玲, 陈小泉, 等. 食品与药品, 2014, 16(4):284
[14] Ai L F, Ma Y S, Chen R C, et al. Chinese Journal of Analytical Chemistry, 2013, 41(8):1194艾连峰, 马育松, 陈瑞春, 等. 分析化学, 2013, 41(8):1194
[15] Bernsmann T, Fürst P, Godula M. Food Addit Contam, 2011, 28(10):1352
[16] Stolker A A M, Peters R J B, Zuiderent R, et al. Anal Bioanal Chem, 2010, 397(7):2841
[17] Zhang L, Kong X H, Wang H, et al. Chinese Journal of Analytical Chemistry, 2014, 42(12):1735张璐, 孔祥虹, 王菡, 等. 分析化学, 2014, 42(12):1735
[18] Couchman L. Biomed Chromatogr, 2012, 26(8):892
[19] Berg T, Lundanes E, Christophersen A S. J Chromatogr B, 2009, 877(4):421
[20] Kasprzyk-Hordem B, Dinsdale R M, Guwy A J. J Chromatogr A, 2007, 1161:132
[21] Wood M, Laloup M, Fernandez M D R, et al. Forensic Sci Int, 2005, 150(2/3):227
[22] Lurie I S, Toske S G. J Chromatogr A, 2008, 1188:322
[23] Matuszewski B K, Constanzer M L, Chavez-Eng C M. Anal Chem, 2003, 75(13):3019  "

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