高效液相色谱-串联质谱法测定功能饮料中肌醇的含量
|
摘要
目的建立液相色谱-串联质谱法测定功能饮料中肌醇的含量。方法功能饮料振荡混匀后取样0.2mL,用50%的乙腈水稀释500倍,过0.22μm的微孔滤膜后直接进样,经BEH Amide色谱柱(2.1mm×100 mm, 1.7μm)洗脱,流动相为乙腈-水,柱温为30℃,流速为0.3 mL/min,用串联四极杆质谱采用多反应监测模式进行测定,外标曲线法定量。结果肌醇在0.05～2.0μg/mL范围内线性关系良好,线性相关系数r为0.9999,检出限和定量限分别为0.65 mg/L和2.15 mg/L;加标浓度为0.025、0.125和0.25 mg/mL的平均回收率分别为103.5%、100.0%和101.8%,批内精密度分别为3.3%、1.1%和1.5%,批间精密度分别为3.3%、2.0%和1.9%。结论该方法前处理简单、快速、准确、灵敏,可以满足实际检测分析的需要。
Objective To establish a method for the determination of inositol in functional drink by high performance liquid chromatography-tandem mass spectrometry. Methods After shaking and mixing, 0.2 mL functional drink was diluted 500 times with 50% acetonitrile water, and directly injected after passing through 0.22 μm microporous membrane filter. Inositol was separated by BEH Amide column(2.1 mm×100 mm, 1.7 μm) with acetonitrile-water as the mobile phase at 30 ℃, and the flow rate was 0.3 mL/min. The sample was determined by tandem quadrupole mass spectrometry using multi-reaction monitoring mode, and quantified by external standard method. Results The inositol had a good linear relationship in the concentration range of 0.05-2.0 μg/mL with correlation coefficients of 0.9999. The limit of detection and limit of quantitative were 0.65 mg/L and 2.15 mg/L, respectively. The average recovery of inositol with the spiked concentration of 0.025, 0.125 and 0.25 mg/mL were 103.5%, 100.0% and 101.8%, the intra-batch precision were 3.3%, 1.1% and 1.5%, and the inter-batch precision were 3.3%、2.0%和1.9%, respectively. Conclusion This method is simple, accurate and sensitive, which can meet the requirements of practical analysis.
Objective To establish a method for the determination of inositol in functional drink by high performance liquid chromatography-tandem mass spectrometry. Methods After shaking and mixing, 0.2 mL functional drink was diluted 500 times with 50% acetonitrile water, and directly injected after passing through 0.22 μm microporous membrane filter. Inositol was separated by BEH Amide column(2.1 mm×100 mm, 1.7 μm) with acetonitrile-water as the mobile phase at 30 ℃, and the flow rate was 0.3 mL/min. The sample was determined by tandem quadrupole mass spectrometry using multi-reaction monitoring mode, and quantified by external standard method. Results The inositol had a good linear relationship in the concentration range of 0.05-2.0 μg/mL with correlation coefficients of 0.9999. The limit of detection and limit of quantitative were 0.65 mg/L and 2.15 mg/L, respectively. The average recovery of inositol with the spiked concentration of 0.025, 0.125 and 0.25 mg/mL were 103.5%, 100.0% and 101.8%, the intra-batch precision were 3.3%, 1.1% and 1.5%, and the inter-batch precision were 3.3%、2.0%和1.9%, respectively. Conclusion This method is simple, accurate and sensitive, which can meet the requirements of practical analysis.
引文
[1]孙灵霞,陈锦屏.肌醇生产、应用研究及前景展望[J].粮食与油脂,2004,(11):6-8.Sun LX,Chen JP.The production application and prospect of inositol[J].Cereal Oil,2004,(11):6-8.
[2]张芹,王芳,陈雅蕾,等.肌醇生产及应用研究进展[J].中国稻米,2012,18(3):19-21.Zhang Q,Wang F,Chen YL,et al.Research progress in inositol production and application[J].China Ric,2012,18(3):19-21.
[3]乔善磊,姜涛,张晓玲,等.气相色谱法及气相色谱-质谱法测定保健饮料中的肌醇[J].中国卫生检验杂志,2009,19(9):2020-2022.Qiao SL,Jiang T,Zhang XL,et al.Determination of inositol in functional beverage by GC-MS and GC-FID[J].Chin J Health Lab Technol,2009,19(9):2020-2022.
[4]None.AOAC SMPR 2012.012:Standard method performance requirements for myo-inositol in infant formula and adult pediatric nutritional formula[J].J AOAC Int,2012,95(2):295.
[5]廖燕芝,黄辉,梁锋.气相色谱法测定婴幼儿配方食品中肌醇的衍生方法的比较[J].食品安全质量检测学报,2018,9(17):4639-4644.Liao YZ,Huang H,Liang F.Comparison of derivative methods for inositol in infant formula foods by gas chromatography[J].J Food Saf Qual,2018,9(17):4639-4644.
[6]刘洪,黄丽彬,刘静.功能饮料现状及新品开发[J].饮料工业,2004,(5):8-10.Liu H,Huang LB,Liu J.Current situation and new product development of functional beverages[J].Bever Ind,2004,(5):8-10.
[7]童晓萌,柴春祥.黄豆荞麦固态饮料配方的优化[J].食品工业科技,2018,39(1):177-182.Tong XM,Chai CX.Optimization of formula of soybean buckwheat solid beverage[J].Sci Technol Food Ind,2018,39(1):177-182.
[8]Greubel S.Isotonic beverages,"energy"and"power"drinks[J].Med Monatsschr Pharm,1998,21(11):353-355.
[9]Oteri AF,Salvo AP,Caputi AP,et al.Intake of energy drinks in association with alcoholic beverages in a cohort of students of the school of medicine of the university of Messina[J].Alcohol Clin Exp Res,2007,31(10):1677-1680.
[10]杜雪莉,饶瑾瑜,张凤枰,等.气相色谱法测定水产预混合饲料中肌醇含量的不确定度评定[J].中国渔业质量与标准,2015,5(5):61-66.Du XL,Rao JY,Zhang FP,et al.Evaluation of uncertainty in determination of inositol in aquatic premixed feed by gas chromatography[J].Chin Fish Qual Stand,2015,5(5):61-66.
[11]安彦新,郭金,王秀伟,等.人血浆肌醇气相色谱质谱联用检测方法的优化及应用[J].中国优生与遗传杂志,2017,25(10):32-35,87.An YX,Guo J,Wang XW,et al.Optimization and application of gas chromatography-mass spectrometry for the determination of inositol in human plasma[J].Chin J Eugeni Genet,2017,25(10):32-35,87.
[12]杨大进,方从容,王竹天.保健食品中肌醇含量测定方法研究[J].中国食品卫生杂志,1999,11(2):9-10.Yang DJ,Fang CR,Wang ZT.Study on determination method of inositol content in health food[J].Chin J Food Hyg,1999,11(2):9-10.
[13]周敏,陈亚波,杨彤.微生物法测定维生素功能饮料中的肌醇含量[J].安徽农业科学,2014,42(7):2123-2125.Zhou M,Chen YB,Yang T.Determination of inositol in vitamin function drinks by microbiological method[J].J Anhui Agric Sci,2014,42(7):2123-2125.
[14]范迪,张梦悦,杨燕,等.微生物法测定食品中的肌醇含量[J].食品安全质量检测学报,2018,9(13):3474-3478.Fan D,Zhang MY,Yang Y,et al.Determination of inositol in food by microbiological method[J].J Food Saf Qual,2018,9(13):3474-3478.
[15]李东飞,于翠霞.功能饮料中肌醇含量的测定方法[J].临床医药文献电子杂志,2017,4(50):9876.Li DF,Yu CX.Determination of inositol in functional beverages[J].J Clin Med,2017,4(50):9876.
[16]曾静,时逸吟,张孝刚,等.固相萃取-气相色谱法测定婴幼儿配方奶粉中肌醇含量[J].检验检疫学刊,2014,24(2):40-43.Zeng J,Shi YY,Zhang XG,et al.Determination of inositol in infant formula by solid phase extraction and gas chromatography[J].J Inspect Quarant,2014,24(2):40-43.
[17]赵凯,孙岚,李玮,等.气相色谱质谱法测定功能性饮料中的肌醇[J].分析试验室,2009,28(S1):122-124.Zhao K,Sun L,Li W,et al.Determination of inositol in functional beverages by gas chromatography[J].Chin J Anal Lab,2009,28(S1):122-124.
[18]招启文,张可冬,陈晓,等.气相色谱-质谱联用测定固体运动饮料中肌醇的含量[J].食品工业,2017,38(7):286-288.Zhao QW,Zhang KD,Chen X,et al.Determination of inositol in solid sports drinks by GC-MS[J].Food Ind,2017,38(7):286-288.
[19]Ruiz-Matute AI,Montilla A,Castillo MDD,et al.A GC method for simultaneous analysis of bornesitol,other polyalcohols and sugars in coffee and its substitutes[J].J Sep Sci,2007,30(4):557-562.
[20]张萍,石波,梁平.离子色谱法快速测定鱼预混饲料中的肌醇[J].现代科学仪器,2005,(1):78-80.Zhang P,Shi B,Liang P.Rapid determination of inositol in fish premix by ion chromatography[J].Mod Sci Instrum,2005,(1):78-80.
[21]戴传波,李建桥,李健秀.示差折光检测法检测肌醇含量[J].食品工业科技,2007,4(62):222-223.Dai CB,Li JQ,Li JX,et al.Differential refraction method for determination of inositol content[J].Food Ind Sci Technol,2007,4(62):222-223.
[22]Cavalli CC,Teng C,Battaglia FC,et al.Free sugar and sugar alcohol concentrations in human breast milk[J].J Pediatr Gastroenterol Nutr,2006,42(2):215-221.
[23]Ellingson DT,Pritchard T,Foy P,et al.Determination of free and total myo-inositol in infant formula and adultpediatric nutritional formula by high-performance anion exchange chromatography with pulsed amperometric detection,including a novel total extraction using microwave-assisted acid hydrolysis and enzymatic treatment:First action2012.12[J].J AOAC Int,2013,96(5):1068-1072.
[24]金梦,谢守新,林海丹,等.婴幼儿配方奶粉中肌醇的液相色谱串联质谱法测定[J].中国乳品工业,2014,42(12):34-36.Jin M,Xie SX,Lin HD,et al.Determination of inositol in infant formula by liquid chromatography and mass spectrometry[J].China Dairy Ind,2014,42(12):34-36.
[25]黄金凤,寻知庆,汪晨霞,等.HPLC-MS/MS法测定婴幼儿配方乳粉中胆碱、左旋肉碱、牛磺酸与肌醇[J].分析测试学报,2018,37(6):702-707.Huang JF,Xun ZQ,Wang CX,et al.Simultaneous determination of choline,L-carnitine,taurine and inositol in infant formula milk powder by HPLC-MS/MS[J].J Instrum Anal,2018,37(6):702-707.
[26]Leung KY,Kmills KA,Burren KA,et al.Quantitative analysis of myo-inositol in urine,blood and nutritional supplements by high-performance liquid chromatography tandem mass spectrometry[J].JChromatogr B Analyt Technol Biomed Life Sci,2011,879(26):2759-2763.
[27]Schimpf KJ,Meek CC,Leff RD,et al.Quantification of myo-inositol,1,5-anhydro-D-sorbitol,and D-chiro-inositol using high-performance liquid chromatography with electrochemical detection in very small volume clinical samples[J].Biomed Chromatogr,2015,29(11):1629-1636.
[28]GB 5009.270-2016食品安全国家标准食品中肌醇的测定[S].GB 5009.270-2016 National food safety standard-Determination of inositol in foods[S].
[29]GB/T 5009.196-2003保健食品中肌醇的测定[S].GB 5009.196-2003 Determination of inositol in health food[S].
[30]向平,沈敏,卓先义.液相色谱-质谱分析中的基质效应[J].分析测试学报,2009,28(6):753-756.Xiang P,Shen M,Zhuo XY.Matrix effects in liquid chromatographic-mass spectrometric analysis[J].J Instrum Anal,2009,28(6):753-756.
[31]李志刚,任男,马燕红,等.高效液相色谱-串联质谱法检测鲜冻肉中违禁注水药物[J].食品科学,2018,39(12):308-312.Li ZG,Ren N,Ma YH,et al.Determination of illegal water-retaining drugs in frozen meat by UPLC-MS/MS[J].Food Sci,2018,39(12):308-312.
[32]Economou A,Botitsi H,Antoniou S,et al.Determination of multi-class pesticides in wines by solid-phase extraction and liquid chromatography-tandem mass spectrometry[J].J Chromatogr A.2009,1216(31):5856-5867.
[2]张芹,王芳,陈雅蕾,等.肌醇生产及应用研究进展[J].中国稻米,2012,18(3):19-21.Zhang Q,Wang F,Chen YL,et al.Research progress in inositol production and application[J].China Ric,2012,18(3):19-21.
[3]乔善磊,姜涛,张晓玲,等.气相色谱法及气相色谱-质谱法测定保健饮料中的肌醇[J].中国卫生检验杂志,2009,19(9):2020-2022.Qiao SL,Jiang T,Zhang XL,et al.Determination of inositol in functional beverage by GC-MS and GC-FID[J].Chin J Health Lab Technol,2009,19(9):2020-2022.
[4]None.AOAC SMPR 2012.012:Standard method performance requirements for myo-inositol in infant formula and adult pediatric nutritional formula[J].J AOAC Int,2012,95(2):295.
[5]廖燕芝,黄辉,梁锋.气相色谱法测定婴幼儿配方食品中肌醇的衍生方法的比较[J].食品安全质量检测学报,2018,9(17):4639-4644.Liao YZ,Huang H,Liang F.Comparison of derivative methods for inositol in infant formula foods by gas chromatography[J].J Food Saf Qual,2018,9(17):4639-4644.
[6]刘洪,黄丽彬,刘静.功能饮料现状及新品开发[J].饮料工业,2004,(5):8-10.Liu H,Huang LB,Liu J.Current situation and new product development of functional beverages[J].Bever Ind,2004,(5):8-10.
[7]童晓萌,柴春祥.黄豆荞麦固态饮料配方的优化[J].食品工业科技,2018,39(1):177-182.Tong XM,Chai CX.Optimization of formula of soybean buckwheat solid beverage[J].Sci Technol Food Ind,2018,39(1):177-182.
[8]Greubel S.Isotonic beverages,"energy"and"power"drinks[J].Med Monatsschr Pharm,1998,21(11):353-355.
[9]Oteri AF,Salvo AP,Caputi AP,et al.Intake of energy drinks in association with alcoholic beverages in a cohort of students of the school of medicine of the university of Messina[J].Alcohol Clin Exp Res,2007,31(10):1677-1680.
[10]杜雪莉,饶瑾瑜,张凤枰,等.气相色谱法测定水产预混合饲料中肌醇含量的不确定度评定[J].中国渔业质量与标准,2015,5(5):61-66.Du XL,Rao JY,Zhang FP,et al.Evaluation of uncertainty in determination of inositol in aquatic premixed feed by gas chromatography[J].Chin Fish Qual Stand,2015,5(5):61-66.
[11]安彦新,郭金,王秀伟,等.人血浆肌醇气相色谱质谱联用检测方法的优化及应用[J].中国优生与遗传杂志,2017,25(10):32-35,87.An YX,Guo J,Wang XW,et al.Optimization and application of gas chromatography-mass spectrometry for the determination of inositol in human plasma[J].Chin J Eugeni Genet,2017,25(10):32-35,87.
[12]杨大进,方从容,王竹天.保健食品中肌醇含量测定方法研究[J].中国食品卫生杂志,1999,11(2):9-10.Yang DJ,Fang CR,Wang ZT.Study on determination method of inositol content in health food[J].Chin J Food Hyg,1999,11(2):9-10.
[13]周敏,陈亚波,杨彤.微生物法测定维生素功能饮料中的肌醇含量[J].安徽农业科学,2014,42(7):2123-2125.Zhou M,Chen YB,Yang T.Determination of inositol in vitamin function drinks by microbiological method[J].J Anhui Agric Sci,2014,42(7):2123-2125.
[14]范迪,张梦悦,杨燕,等.微生物法测定食品中的肌醇含量[J].食品安全质量检测学报,2018,9(13):3474-3478.Fan D,Zhang MY,Yang Y,et al.Determination of inositol in food by microbiological method[J].J Food Saf Qual,2018,9(13):3474-3478.
[15]李东飞,于翠霞.功能饮料中肌醇含量的测定方法[J].临床医药文献电子杂志,2017,4(50):9876.Li DF,Yu CX.Determination of inositol in functional beverages[J].J Clin Med,2017,4(50):9876.
[16]曾静,时逸吟,张孝刚,等.固相萃取-气相色谱法测定婴幼儿配方奶粉中肌醇含量[J].检验检疫学刊,2014,24(2):40-43.Zeng J,Shi YY,Zhang XG,et al.Determination of inositol in infant formula by solid phase extraction and gas chromatography[J].J Inspect Quarant,2014,24(2):40-43.
[17]赵凯,孙岚,李玮,等.气相色谱质谱法测定功能性饮料中的肌醇[J].分析试验室,2009,28(S1):122-124.Zhao K,Sun L,Li W,et al.Determination of inositol in functional beverages by gas chromatography[J].Chin J Anal Lab,2009,28(S1):122-124.
[18]招启文,张可冬,陈晓,等.气相色谱-质谱联用测定固体运动饮料中肌醇的含量[J].食品工业,2017,38(7):286-288.Zhao QW,Zhang KD,Chen X,et al.Determination of inositol in solid sports drinks by GC-MS[J].Food Ind,2017,38(7):286-288.
[19]Ruiz-Matute AI,Montilla A,Castillo MDD,et al.A GC method for simultaneous analysis of bornesitol,other polyalcohols and sugars in coffee and its substitutes[J].J Sep Sci,2007,30(4):557-562.
[20]张萍,石波,梁平.离子色谱法快速测定鱼预混饲料中的肌醇[J].现代科学仪器,2005,(1):78-80.Zhang P,Shi B,Liang P.Rapid determination of inositol in fish premix by ion chromatography[J].Mod Sci Instrum,2005,(1):78-80.
[21]戴传波,李建桥,李健秀.示差折光检测法检测肌醇含量[J].食品工业科技,2007,4(62):222-223.Dai CB,Li JQ,Li JX,et al.Differential refraction method for determination of inositol content[J].Food Ind Sci Technol,2007,4(62):222-223.
[22]Cavalli CC,Teng C,Battaglia FC,et al.Free sugar and sugar alcohol concentrations in human breast milk[J].J Pediatr Gastroenterol Nutr,2006,42(2):215-221.
[23]Ellingson DT,Pritchard T,Foy P,et al.Determination of free and total myo-inositol in infant formula and adultpediatric nutritional formula by high-performance anion exchange chromatography with pulsed amperometric detection,including a novel total extraction using microwave-assisted acid hydrolysis and enzymatic treatment:First action2012.12[J].J AOAC Int,2013,96(5):1068-1072.
[24]金梦,谢守新,林海丹,等.婴幼儿配方奶粉中肌醇的液相色谱串联质谱法测定[J].中国乳品工业,2014,42(12):34-36.Jin M,Xie SX,Lin HD,et al.Determination of inositol in infant formula by liquid chromatography and mass spectrometry[J].China Dairy Ind,2014,42(12):34-36.
[25]黄金凤,寻知庆,汪晨霞,等.HPLC-MS/MS法测定婴幼儿配方乳粉中胆碱、左旋肉碱、牛磺酸与肌醇[J].分析测试学报,2018,37(6):702-707.Huang JF,Xun ZQ,Wang CX,et al.Simultaneous determination of choline,L-carnitine,taurine and inositol in infant formula milk powder by HPLC-MS/MS[J].J Instrum Anal,2018,37(6):702-707.
[26]Leung KY,Kmills KA,Burren KA,et al.Quantitative analysis of myo-inositol in urine,blood and nutritional supplements by high-performance liquid chromatography tandem mass spectrometry[J].JChromatogr B Analyt Technol Biomed Life Sci,2011,879(26):2759-2763.
[27]Schimpf KJ,Meek CC,Leff RD,et al.Quantification of myo-inositol,1,5-anhydro-D-sorbitol,and D-chiro-inositol using high-performance liquid chromatography with electrochemical detection in very small volume clinical samples[J].Biomed Chromatogr,2015,29(11):1629-1636.
[28]GB 5009.270-2016食品安全国家标准食品中肌醇的测定[S].GB 5009.270-2016 National food safety standard-Determination of inositol in foods[S].
[29]GB/T 5009.196-2003保健食品中肌醇的测定[S].GB 5009.196-2003 Determination of inositol in health food[S].
[30]向平,沈敏,卓先义.液相色谱-质谱分析中的基质效应[J].分析测试学报,2009,28(6):753-756.Xiang P,Shen M,Zhuo XY.Matrix effects in liquid chromatographic-mass spectrometric analysis[J].J Instrum Anal,2009,28(6):753-756.
[31]李志刚,任男,马燕红,等.高效液相色谱-串联质谱法检测鲜冻肉中违禁注水药物[J].食品科学,2018,39(12):308-312.Li ZG,Ren N,Ma YH,et al.Determination of illegal water-retaining drugs in frozen meat by UPLC-MS/MS[J].Food Sci,2018,39(12):308-312.
[32]Economou A,Botitsi H,Antoniou S,et al.Determination of multi-class pesticides in wines by solid-phase extraction and liquid chromatography-tandem mass spectrometry[J].J Chromatogr A.2009,1216(31):5856-5867.