QuEChERS法结合液相色谱-串联质谱测定保健食品中50种非食用添加物
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摘要
建立了液相色谱-串联质谱法测定保健食品中50种非食用添加物的分析方法。样品经甲醇提取,QuEChERS法净化,Agilent Phoroshell SB C_(18)柱(150 mm×3.0 mm, 2.7μm)分离,并以0.1%(v/v)甲酸水溶液与乙腈为流动相,梯度洗脱,电喷雾正离子模式和负离子模式同时扫描,多反应监测模式(MRM)检测。结果表明,50种化合物均得到较好的分离,线性范围内基质匹配标准溶液的线性关系良好(r~2>0.99)。方法的检出限(LOD,S/N≥3)与定量限(LOQ,S/N≥10)分别为0.010～1 mg/kg和0.02～2 mg/kg。考察了50种非食用添加物在5种典型保健食品基质(口服液、片剂、膏剂、丸剂、胶囊)中的加标回收率,在1 LOQ、2 LOQ、10 LOQ加标水平的平均回收率为63.1%～115.7%,相对标准偏差(RSD)均不大于8.9%(n=6)。该方法简单、灵敏度高且实用性强,适用于保健食品中50种非食用添加物的确证。
A liquid chromatography-tandem mass spectrometry(LC-MS/MS) method was established for the determination of 50 non-food additives in health food. The samples were extracted with methanol and purified using the QuEChERS method. The separation was performed on an Agilent Phoroshell SB C_(18) column(150 mm×3.0 mm, 2.7 μm) with a mobile phase of 0.1%(v/v) formic acid aqueous solution and acetonitrile. The determination was performed by MS/MS in positive or negative electrospray ionization and multiple reaction monitoring mode. The results demonstrated that all 50 compounds could be well separated with a good linear relationship(r~2>0.99). The limits of detection(LODs, S/N≥3) and limits of quantification(LOQs, S/N≥10) were in the range of 0.010-1 mg/kg and 0.020-2 mg/kg, respectively. The matrix effects in five kinds of typical health foods(oral liquid, tablets, ointments, pills, and capsules) were evaluated and reduced by means of matrix matching. At the spiked levels of 1 LOQ, 2 LOQ, and 10 LOQ, the recoveries of all drugs varied from 63.1% to 115.7% with relative standard deviations(RSDs) of no more than 8.9%(n=6). The method is simple, sensitive, practical, and suitable for monitoring 50 non-edible additives in health food.
A liquid chromatography-tandem mass spectrometry(LC-MS/MS) method was established for the determination of 50 non-food additives in health food. The samples were extracted with methanol and purified using the QuEChERS method. The separation was performed on an Agilent Phoroshell SB C_(18) column(150 mm×3.0 mm, 2.7 μm) with a mobile phase of 0.1%(v/v) formic acid aqueous solution and acetonitrile. The determination was performed by MS/MS in positive or negative electrospray ionization and multiple reaction monitoring mode. The results demonstrated that all 50 compounds could be well separated with a good linear relationship(r~2>0.99). The limits of detection(LODs, S/N≥3) and limits of quantification(LOQs, S/N≥10) were in the range of 0.010-1 mg/kg and 0.020-2 mg/kg, respectively. The matrix effects in five kinds of typical health foods(oral liquid, tablets, ointments, pills, and capsules) were evaluated and reduced by means of matrix matching. At the spiked levels of 1 LOQ, 2 LOQ, and 10 LOQ, the recoveries of all drugs varied from 63.1% to 115.7% with relative standard deviations(RSDs) of no more than 8.9%(n=6). The method is simple, sensitive, practical, and suitable for monitoring 50 non-edible additives in health food.
引文
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[3] Canadian Food Inspection Agency.Foods or Natural Health Products.(2017-10-27) [2019-01-22].http://www.inspection.gc.ca/food/labelling/former-food-labelling-for-industry/former-health-claims/eng/1514559099172/1514559100331 chap=3
[4] Ministry of Health,Labour and Welfare.Correct Usage of Health Food.[2019-01-22].https://www.mhlw.go.jp/topics/bukyoku/iyaku/syoku-anzen/dl/kenkou_shokuhin00.pdf
[5] European Commission.Safety of Food Supplements-Commissioner Byrne Welcomes Political Agreement in Council.(2001-09-27) [2019-01-22].http://europa.eu/rapid/press-release_IP-01-1324_en.htm
[6] National People’s Congress Standing Committee.Food Safety Law of the People’s Republic of China,Part 5.Beijing:China Legal Publishing House,2015 全国人民代表大会常务委员会.中华人民共和国食品安全法(五).北京:中国法制出版社,2015
[7] SN/T 3867-2014
[8] SN/T 3864-2014
[9] SN/T 4054-2014
[10] Li Y,Xue F,Wang Y,et al.Chinese Journal of Analytical Chemistry,2011,39(11):1716 李阳,薛丰,王媛,等.分析化学,2011,39(11):1716
[11] Li Y,Zhang H,Hu J T,et al.J Chromatogr Sci,2012,50(10):928
[12] Mokhtar S U,Chin S T,Kee C L,et al.J Pharmaceut Biomed Anal,2016,121:188
[13] Lee E S,Lee J H,Han K M,et al.J Pharmaceut Biomed Anal,2013,83(1):171
[14] Kim J Y,Park H J,Kim J W,et al.Arch Pharm Res,2016,39(1):103
[15] Huang F,Wu H Q,Huang X L,et al.Chinese Journal of Chromatography,2016,34(3):270 黄芳,吴惠琴,黄晓兰,等.色谱,2016,34(3):270
[16] Zhong Y,Sun C,Xiong J,et al.J Liq Chromatogr R T,2017,40(12):640
[17] Ding B,Wang Z Y,Xie J J,et al.Chinese Journal of Chromatography,2016,34(6):583 丁博,王志元,谢建军,等.色谱,2016,34(6):583
[18] Yu H,Hu Q,Sun J,et al.Chinese Journal of Chromatography,2018,36(10):1005 于泓,胡青,孙健,等.色谱,2018,36(10):1005
[19] Shanghai Municipal Food and Drug Administration.DB 31/2010-2012.(2012-10-26) [2019-01-22].http://file4.foodmate.net/foodvip/web/viewer.html?file=./zengbu/DB 312010-2012.pdf 上海市食品药品监督管理局.DB 31/2010-2012.(2012-10-26) [2019-01-22].http://file4.foodmate.net/foodvip/web/viewer.html?file=./zengbu/DB312010-2012.pdf
[20] Li D,Wen H M,Cui F C,et al.Chinese Journal of Pharmaceutical Analysis,2010,30(8):1527 李丹,文红梅,崔福春,等.药物分析杂志,2010,30(8):1527
[21] Zhu W X,Liu Y F,Sun Z L,et al.Physical Testing and Chemical Analysis Part B:Chemical Analysis,2016,52(11):1286 祝伟霞,刘亚风,孙转莲,等.理化检验-化学分册,2016,52(11):1286
[22] Zheng J,Xi C X,Cao S R,et al.Chinese Journal of Chromatography,2017,35(12):1257 郑佳,郗存显,曹淑瑞,等.色谱,2017,35(12):1257
[23] AOAC International.AOAC Official Method 2007.01.[2019-01-22].https://nucleus.iaea.org/sites/fcris/Shared%20Documents/SOP/AOAC_2007_01.pdf#search=AOAC%20Official%20Method%202007%2E01%2C%20Pesticide%20Residues%20in%20Foods%20by%20Acetonitrile%20 Extraction%20and%20Partitioning%20with%20Magnesium %20Sulfate%2C%202007%2E
[24] British Standards Institution.BS EN 15662:2008.[2019-01-22].http://www.chromnet.net/Taiwan/QuEChERS_Dispersive_SPE/QuEChERS_%E6%AD%90%E7%9B%9F%E6%96%B9%E6%B3%95_EN156622008_E.pdf
[25] Liu F J,Guo X D,Weng Y B,et al.Journal of Instrumental Analysis,2014,33(3):329 刘付建,郭新东,翁乙斌,等.分析测试学报,2014,33(3):329
[26] Chen J J,Zhang J,Wu S Z,et al.Chinese Journal of Chromatography,2016,34(10):1005 陈姣姣,张静,吴思卓,等.色谱,2016,34(10):1005
[27] Zhao L,Lucas D,Long D,et al.J Chromatogr A,2018,1549:14
[28] Qin L,Dong Y L,Wang G L,et al.Chinese Journal of Chromatography,2018,36(9):880 覃玲,董亚蕾,王钢力,等.色谱,2018,36(9):880
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