LU Hui, QIAN Ye-fei, ZHANG Bin, HAO Gang, CHEN Li-bo. Determination of rhubarb anthraquinones and illegally added chemical drugs in weight- loss functional foods[J]. Science and Technology of Food Industry, 2016, (10): 88-93. DOI: 10.13386/j.issn1002-0306.2016.10.008

Citation: LU Hui, QIAN Ye-fei, ZHANG Bin, HAO Gang, CHEN Li-bo. Determination of rhubarb anthraquinones and illegally added chemical drugs in weight- loss functional foods[J]. Science and Technology of Food Industry, 2016, (10): 88-93. DOI: 10.13386/j.issn1002-0306.2016.10.008

減肥類保健食品中蒽醌類成分及非法添加化學(xué)藥物的測(cè)定

詳細(xì)信息

作者簡(jiǎn)介:

魯輝(1982-),男,碩士,主管藥師,研究方向:保健食品、化妝品檢測(cè)與質(zhì)量控制,E-mail:15862509876@163.com。;

陳麗波(1969-),女,主任藥師,主要從事保健食品、化妝品質(zhì)量控制與評(píng)價(jià)方面的研究,E-mail:chenlb@szifdc.org.cn。;

中圖分類號(hào): TS218;O657

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Determination of rhubarb anthraquinones and illegally added chemical drugs in weight- loss functional foods

Suzhou Institute for Food and Drug Control

摘要

摘要: 建立同時(shí)測(cè)定減肥類保健食品中非法添加化學(xué)藥物氟西汀、比沙可啶以及蒽醌類成分番瀉苷A、番瀉苷B、大黃素、大黃素甲醚、大黃酸、大黃酚、蘆薈苷和蘆薈大黃素的高效液相色譜-二極管陣列檢測(cè)器（HPLC-DAD）方法。采用Diamonsil C18色譜柱（250 mm×4.6 mm,5μm）,以乙腈（A）-0.02 mol/L乙酸銨溶液（含0.4%乙酸）（B）為流動(dòng)相,梯度洗脫（05 min,85%B;525 min,85%B35%B;2550 min,35%B;5055 min,35%B85%B）,測(cè)定波長(zhǎng)為268 nm,流速1.0 m L/min,柱溫25℃。對(duì)HPLC-DAD檢出氟西汀和比沙可啶的樣品進(jìn)行電噴霧飛行時(shí)間質(zhì)譜（ESI-Q-TOF/MS）一級(jí)掃描及二級(jí)碎片離子比對(duì)進(jìn)行陽(yáng)性確證。結(jié)果表明:10種待測(cè)物線性關(guān)系良好（r≥0.995）,平均回收率位于90.3%104.7%之間,RSD均小于5.0%。實(shí)際樣品測(cè)定發(fā)現(xiàn)25種減肥類保健食品中有2種檢出氟西汀,1種檢出比沙可啶,另有1種樣品同時(shí)檢出蘆薈苷和蘆薈大黃素。本文建立的方法具有較高的選擇性和靈敏度,方法分離效果好,耐用性較強(qiáng),能夠用于減肥類保健食品中這10種成分的定性、定量測(cè)定。 

Abstract: An analytical method using high performance liquid chromatography coupled with diode array detector( HPLC- DAD) was developed for determination of illegally added chemical drugs fluoxetine and bisacodyl,and rhubarb anthraquinones such as sennoside A,sennoside B,emodin,emodin monomethyl ether,rheinic acid,chrysophanol,barbaloin and aloe- emodin in weight- loss functional foods. The separation was performed on a Diamonsil C18column( 250 mm × 4.6 mm,5 μm) by gradient elution of acetonitril and 0.02 mol / L ammonium acetate solution( containing 0.4% acetic acid) at a flow rate of 1.0 m L / min: 0~5 min,85% B,5~25 min,85% B~35% B,25~50 min,35% B,50~55 min,35% B~85% B.The detection wavelength was 268 nm and the column temperature was25 ℃. The samples containing fluoxetine or bisacodyl were confirmed by two grade of fragmention comparison using electrospray ionization- quadrupole- time of flight mass spectrometer( ESI- Q- TOF/ MS). The correlation coefficient of standard curve for each component in linearity range was not less than 0.995,as well as the average recoveries were 90.3% ~ 104.7% with the relative standard deviations( RSDs) were not more than 5.0%. After determination of 25 weight- loss functional foods,the fluoxetine and bisacodyl were detected in 2 and 1 samples,respectively.The barbaloin and aloe- emodin were both detected in one of the 25 samples.The method is reliable,sensitive,accurate and reproducible.It can be used for the qualitative and quantitative determination of above 10 components in weight- loss functional foods.

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參考文獻(xiàn)(11)

[1] 孫鑫貴,趙榕,張正,等.2005-2008年全國(guó)減肥類保健食品違法添加藥物狀況調(diào)查及分析[J].中國(guó)食品衛(wèi)生雜志,2010,22(5):453-455. [2] 王靜文,黃湘鷺,曹進(jìn),等.超高效液相色譜法同時(shí)測(cè)定減肥類保健食品中非法添加的25種藥物[J].色譜,2014,32(2):151-156. [3] 國(guó)家食品藥品監(jiān)督管理局.藥品檢驗(yàn)補(bǔ)充檢驗(yàn)方法和檢驗(yàn)項(xiàng)目批準(zhǔn)件2006004[S].2006. [4] 國(guó)家食品藥品監(jiān)督管理局.食藥監(jiān)辦許[2010]114號(hào)文件附件2:減肥類保健食品違法添加藥物的檢測(cè)方法[S].2010. [5] 國(guó)家食品藥品監(jiān)督管理局.藥品檢驗(yàn)補(bǔ)充檢驗(yàn)方法和檢驗(yàn)項(xiàng)目批準(zhǔn)件2012005[S].2012. [6] 肖晶,楊杰,高尚偉,等.HPLC法測(cè)定保健食品中蒽醌類成分的含量[J].中國(guó)食品衛(wèi)生雜志,2010,22(1):27-30. [7] 汪鳳云,李紅艷,鞏飚.HPLC法測(cè)定蘆薈保健制品中蘆薈苷的含量[J].中國(guó)衛(wèi)生檢驗(yàn)雜志,2008,18(11):2238-2239. [8] 莫紫梅,朱斌.高效液相色譜法測(cè)定保健食品中番瀉苷含量的研究[J].中國(guó)衛(wèi)生檢驗(yàn)雜志,2014,24(5):2238-2239. [9] 余翠琴,張凡.慎用瀉藥[J].中國(guó)臨床藥學(xué)雜志,2002,11(5):307-308. [10] 李軍生,鄒義英.蘆薈類保健食品的毒理學(xué)安全性評(píng)價(jià)[J].毒理學(xué)雜志,2009,23(3):253-254. [11] 李衛(wèi)東.長(zhǎng)期應(yīng)用番瀉葉對(duì)大鼠結(jié)腸電及Cajal間質(zhì)細(xì)胞的影響[J].廣州中醫(yī)藥大學(xué)學(xué)報(bào),2005,22(5):408-409.

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