超高效液相色谱-串联质谱法测定米粉和河粉中的米酵菌酸
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摘要
目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定河粉和米粉中米酵菌酸(bongkrekic acid, BA)的含量。方法试样经提取、净化、浓缩及过滤后,以0.1%甲酸水和乙腈作为流动相进行梯度洗脱,采用电喷雾离子源负模式检测,外标法定量。基于米酵菌酸色谱和质谱行为的研究,对其仪器测定条件进行优化,并对优化后的方法进行方法学验证。结果米酵菌酸在1～100μg/L浓度范围内线性良好,相关系数大于0.999。在2种基质不同加标浓度下,回收率80.6%～104.8%,相对标准偏差小于5%。米酵菌酸在2种基质中的检出限为0.1μg/kg,定量限为0.2μg/kg。结论方法灵敏度高、专属性好、准确可靠,适用于米粉和河粉基质中米酵菌酸的测定。
Objective To establish a method for the determination of bongkrekic acid(BA) in rice noodles and fried rice noodles by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods After the samples were extracted, purified, concentrated and filtered, 0.1% formic acid water and acetonitrile were used as mobile phase for gradient elution. The samples were detected by electrospray ion source negative mode(ESI-)and quantified by external standard method. Based on the study of the chromatographic and mass spectrometric behaviors of BA, the conditions of its instrumental determination were optimized, and the optimized method was validated. Results BA had a good linearity in the concentration range of 1-100 μg/L, and the correlation coefficient was greater than 0.999. Under the different spiked concentrations of two substrates, the recoveries were 80.6%-104.8%,with the relative standard deviations were less than 5%. The limits of detection of 2 matrices were 0.1 μg/kg, and the limits of quantification were 0.2 μg/kg. Conclusion This method has high sensitivity, good specificity, accuracy and reliability, which is suitable for the determination of BA in rice noodles and fried rice noodles.
Objective To establish a method for the determination of bongkrekic acid(BA) in rice noodles and fried rice noodles by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods After the samples were extracted, purified, concentrated and filtered, 0.1% formic acid water and acetonitrile were used as mobile phase for gradient elution. The samples were detected by electrospray ion source negative mode(ESI-)and quantified by external standard method. Based on the study of the chromatographic and mass spectrometric behaviors of BA, the conditions of its instrumental determination were optimized, and the optimized method was validated. Results BA had a good linearity in the concentration range of 1-100 μg/L, and the correlation coefficient was greater than 0.999. Under the different spiked concentrations of two substrates, the recoveries were 80.6%-104.8%,with the relative standard deviations were less than 5%. The limits of detection of 2 matrices were 0.1 μg/kg, and the limits of quantification were 0.2 μg/kg. Conclusion This method has high sensitivity, good specificity, accuracy and reliability, which is suitable for the determination of BA in rice noodles and fried rice noodles.
引文
[1]Garcia RA,Hotchkiss JH,Steinkraus KH.The effect of lipids on bongkrekic(bongkrek)acid toxin production by Burkholderia cocovenenans in coconut media[J].Food Addit Contam,1999,16(2):63-69.
[2]Liu X.Microbiology risk assessment in China:current situation and challenges[EB/OL].[2002-07-24].http://foodrisk.org/default/assets/File/IRAC-event-Liu.pdf
[3]Deshpande SS.Bongkrek toxins.In:Handbook of food toxicology[M].New York:Marcel Decker,2002.
[4]Burkholderia cocovenenans foodborne illness-Indonesia[EB/OL].http://www.promedmail.org.
[5]Suspected tempe poisoning,1 killed and 3 treated[EB/OL].[2013-02-15].http://news.okezone.com/read/2013/02/15/513/762277/diduga-keracunan-t empe-1-orang-tewas-3-dirawat.
[6]Meng Z,Li Z,Jin J,et al.Studies on fermented corn flour poisoning in rural areas of China.I.Epidemiology,clinical manifestations,and pathology[J].Biomed Environ Sci,1998,1(1):101-104.
[7]Ramzy A.5 die from food poisoning from southern Chinese snack[EB/OL].[2017-07-04].http://sinosphere.blogs.nytimes.com/2014/07/04/5-die-in-foodpoisoning-from-southern-chinesesnack/?_r=0.
[8]Shen Y,Liu J,Huang Z.Epidemiological analysis of food poisoning due to contamination of fermented flour with Pseudomonas cocovenenans subsp,farino fermentans in Guangxi[J].China Trop Med,2007,7(5):814-815.
[9]Gudo ES,Cook K,Kasper AM,et al.Description of a mass poisoning in a rural district in mozambique:The First documented bongkrekic acid poisoning in Africa[J].Clin Infect Dis,2018,66(9):1400-1406.
[10]Mehruba A,Amelia K,Alaina R,et al.Bongkrekic acid-A review of a lesser-known mitochondrial toxin[J].J Med Toxicol,2017,(13):173-179.
[11]GB 5009.189-2016食品安全国家标准食品中米酵菌酸的测定[S].GB 5009.189-2016 National food safety standard-Determination of yeast acid in food[S].
[12]周霞,陈万勤,傅红雪,等.全自动固相萃取-超高效液相色谱法快速测定食品中米酵菌酸含量[J].安徽农业科学,2018,46(8):159-160,182.Zhou X,Chen WQ,Fu HX,et al.Fast determination of bongkrekic acid in food by auto solid phase extraction-ultra high performance liquid chromatography[J].J Anhui Agric Sci,2018,46(8):159-160,182.
[13]李红艳,金燕飞,黄海智,等.高效液相色谱-二极管阵列检测器结合固相萃取法快速测定食品中米酵菌酸残留[J].食品科学,2016,24(37):247-251.Li HY,Jin YF,Huang HZ,et al.Fast Determination of bongkrekic acid in foods using mixed-mode weak anion exchange solid phase extraction coupled with high performance liquid chromatography with diode array detection(HPLC-DAD)[J].Food Sci,2016,24(37):247-251.
[14]周鹏.超高效液相色谱串联质谱法测定银耳中米酵菌酸[J].食品研究与开发,2015,36(22):123-125.Zhou P.Determination of bongkrekic acid in tremella fuciformis berk by ultra high performance liquid chromatography-tandem mass spectrometry[J].Food Res Dev,2015,36(22):123-125.
[15]苏肯明,梁达清.液相色谱-串联质谱法测定银耳中的米酵菌酸[J].广东化工,2014,41(282):168-169.Su KM,Liang DQ.Determination of bongkrekic acid in Tremella fuciformis by LC-MS/MS[J].Guangzhou Chem Ind Technol,2014,41(282):168-169.
[16]李红娜,袁飞,张辰陽,等.液相色谱和飞行时间质谱联用检测米酵菌酸[J].食品工业,2018,39(7):319-323Li HN,Yuan F,Zhang CY,et al.The research of detection bongkrekic acid(BA)by LC-ESI-TOF technology[J].Food Ind,2018,39(7):319-323.
[2]Liu X.Microbiology risk assessment in China:current situation and challenges[EB/OL].[2002-07-24].http://foodrisk.org/default/assets/File/IRAC-event-Liu.pdf
[3]Deshpande SS.Bongkrek toxins.In:Handbook of food toxicology[M].New York:Marcel Decker,2002.
[4]Burkholderia cocovenenans foodborne illness-Indonesia[EB/OL].http://www.promedmail.org.
[5]Suspected tempe poisoning,1 killed and 3 treated[EB/OL].[2013-02-15].http://news.okezone.com/read/2013/02/15/513/762277/diduga-keracunan-t empe-1-orang-tewas-3-dirawat.
[6]Meng Z,Li Z,Jin J,et al.Studies on fermented corn flour poisoning in rural areas of China.I.Epidemiology,clinical manifestations,and pathology[J].Biomed Environ Sci,1998,1(1):101-104.
[7]Ramzy A.5 die from food poisoning from southern Chinese snack[EB/OL].[2017-07-04].http://sinosphere.blogs.nytimes.com/2014/07/04/5-die-in-foodpoisoning-from-southern-chinesesnack/?_r=0.
[8]Shen Y,Liu J,Huang Z.Epidemiological analysis of food poisoning due to contamination of fermented flour with Pseudomonas cocovenenans subsp,farino fermentans in Guangxi[J].China Trop Med,2007,7(5):814-815.
[9]Gudo ES,Cook K,Kasper AM,et al.Description of a mass poisoning in a rural district in mozambique:The First documented bongkrekic acid poisoning in Africa[J].Clin Infect Dis,2018,66(9):1400-1406.
[10]Mehruba A,Amelia K,Alaina R,et al.Bongkrekic acid-A review of a lesser-known mitochondrial toxin[J].J Med Toxicol,2017,(13):173-179.
[11]GB 5009.189-2016食品安全国家标准食品中米酵菌酸的测定[S].GB 5009.189-2016 National food safety standard-Determination of yeast acid in food[S].
[12]周霞,陈万勤,傅红雪,等.全自动固相萃取-超高效液相色谱法快速测定食品中米酵菌酸含量[J].安徽农业科学,2018,46(8):159-160,182.Zhou X,Chen WQ,Fu HX,et al.Fast determination of bongkrekic acid in food by auto solid phase extraction-ultra high performance liquid chromatography[J].J Anhui Agric Sci,2018,46(8):159-160,182.
[13]李红艳,金燕飞,黄海智,等.高效液相色谱-二极管阵列检测器结合固相萃取法快速测定食品中米酵菌酸残留[J].食品科学,2016,24(37):247-251.Li HY,Jin YF,Huang HZ,et al.Fast Determination of bongkrekic acid in foods using mixed-mode weak anion exchange solid phase extraction coupled with high performance liquid chromatography with diode array detection(HPLC-DAD)[J].Food Sci,2016,24(37):247-251.
[14]周鹏.超高效液相色谱串联质谱法测定银耳中米酵菌酸[J].食品研究与开发,2015,36(22):123-125.Zhou P.Determination of bongkrekic acid in tremella fuciformis berk by ultra high performance liquid chromatography-tandem mass spectrometry[J].Food Res Dev,2015,36(22):123-125.
[15]苏肯明,梁达清.液相色谱-串联质谱法测定银耳中的米酵菌酸[J].广东化工,2014,41(282):168-169.Su KM,Liang DQ.Determination of bongkrekic acid in Tremella fuciformis by LC-MS/MS[J].Guangzhou Chem Ind Technol,2014,41(282):168-169.
[16]李红娜,袁飞,张辰陽,等.液相色谱和飞行时间质谱联用检测米酵菌酸[J].食品工业,2018,39(7):319-323Li HN,Yuan F,Zhang CY,et al.The research of detection bongkrekic acid(BA)by LC-ESI-TOF technology[J].Food Ind,2018,39(7):319-323.