婴幼儿配方乳粉中维生素K1的检测
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摘要
研究了高效液相色谱法检测婴幼儿配方乳粉中维生素K1的关键技术。该方法利用脂肪酶降解试样中的不饱和脂肪酸,经碱皂化,采用正己烷提取,饱和氯化钠(含酚酞溶液)水洗至中性后,再进行浓缩处理,最后用甲醇进行复溶。以甲醇(含冰醋酸、氯化锌和无水乙酸钠)为流动相,通过反相C18色谱柱分离,锌粉还原柱柱后衍生,荧光检测器检测,外标法定量。实验结果表明:维生素K1在0.2~5μg/m L范围内线性关系良好(r≥0.999);添加浓度在5~100μg/100 g时,平均回收率为90%~110%;对三个不同含量的样品进行6次独立测定,其相对标准偏差均小于5%;最低检出限为1μg/100 g。该方法操作简单,结果准确,重复性好,可为企业质量控制和政府监管提供有力的技术支撑。
Key technology research was developed for the determination of vitamin K1 in infant formula by high performance liquid chromatography( HPLC).The sample was enzymatic hydrolysis by lipase,saponified with alkali,and then extracted with hexane,washed with Na Cl saturated solution( containing phenolphthalein solution),and finally,Vitamin K1 was redissolved in methanol.The vitamin K1 were separated on a symmetry C18 column( contecting to the zinc riduction column),and detected with fluorescence detection by the mobile phases of methanol dissolving Zinc chloride,sodium acetate and glacial acetic acid. The result show that the linearity of vitamin K1 was in the concentration ranges of 0.2 to 5 μg/m L,with the good correlation coefficients( r≥0.999).When the concentration of VK,was 5~100 μg/100 g,The average recoveries for the target compounds were between 90% ~110%,6 independent determinations of samples with different contents were carried out with RSD less than5%.The limit of detection was 1 μg/100 g. The method was easy,accurate and highly reproducible,which could provide strong technical support for enterprise quality control and government regulation.
Key technology research was developed for the determination of vitamin K1 in infant formula by high performance liquid chromatography( HPLC).The sample was enzymatic hydrolysis by lipase,saponified with alkali,and then extracted with hexane,washed with Na Cl saturated solution( containing phenolphthalein solution),and finally,Vitamin K1 was redissolved in methanol.The vitamin K1 were separated on a symmetry C18 column( contecting to the zinc riduction column),and detected with fluorescence detection by the mobile phases of methanol dissolving Zinc chloride,sodium acetate and glacial acetic acid. The result show that the linearity of vitamin K1 was in the concentration ranges of 0.2 to 5 μg/m L,with the good correlation coefficients( r≥0.999).When the concentration of VK,was 5~100 μg/100 g,The average recoveries for the target compounds were between 90% ~110%,6 independent determinations of samples with different contents were carried out with RSD less than5%.The limit of detection was 1 μg/100 g. The method was easy,accurate and highly reproducible,which could provide strong technical support for enterprise quality control and government regulation.
引文
[1]王丽杰,孙莹.晚发性维生素K缺乏致颅内出血患儿的临床特征分析[J].中国医科大学学报,2014,43(10):946-949.
[2]席晓芳,朱继红.获得性维生素K依赖性疑血因子缺乏症的病因和治夕创深讨[J].中国医刊,2009,44(4):33-34.
[3]万国堂,苏桂华.口服维生素Kl预防婴儿维生素K缺乏症的效果观察[J].中华儿童保健杂志1995,3(4):245-246.
[4]Anewbornmerican Academy of Pediatrics Committee on Fetus and Newborn.Controversies concerning vitamin K and the newborn[J].Pediatrics,2003,112:191-192.
[5]Shiqing Songa,Xiaoming Zhanga,Khizar Hayat,et al.Contribution of beef base to aroma characteristics of beeflike process flavour assessed by descriptive sebsory analysis and gas chromatography olfactometry and partial least squares regression[J].Journal of Chromatography A,2010,1217(49):7788-7799.
[6]李向荣.绿色蔬菜中维生素K1的薄层_紫外分光光度法测定[J].中国公共卫生,1996,12(8):246.
[7]赵建国,耿聪,齐懿鸣.乳粉中维生素K1高效液相色谱测定方法的改进[J].分析测试技术与仪器,2005,11(4):311-313.
[8]聂西度.高效液相色谱法测定谷物中维生素Kl的含量[J].食品研究与开发,2005,26(4):130-131.
[9]谭建华,席绍峰.高效液相色谱法测定化妆品中的维生素K1[J].分析测试学报.2012,31(11):1451-1454.
[10]邓峰,周英田.高效液相色谱法对食品中维生素K1的定量测定[J].色谱,1996,14(3):233-234.
[11]郝岩平,刘波.乳品中维生素K1的测定[J].中国乳品工业,2003,31(1):30-31.
[12]铁晓威.高效液相色谱柱后衍生法测定食品中的VK1[J].食品与发酵工业,2002,28(9):34-37.
[13]姜瑞清.对GB 5413.10-2010中维生素K1检测的改进研究.中国乳品工业,2011,39(9):50-52.
[14]GB 5413.10-2010婴幼儿食品和乳品中维生素K1的测定[S].
[15]GB 5009.158-2016食品安全国家标准食品中维生素K1的测定[S].
[2]席晓芳,朱继红.获得性维生素K依赖性疑血因子缺乏症的病因和治夕创深讨[J].中国医刊,2009,44(4):33-34.
[3]万国堂,苏桂华.口服维生素Kl预防婴儿维生素K缺乏症的效果观察[J].中华儿童保健杂志1995,3(4):245-246.
[4]Anewbornmerican Academy of Pediatrics Committee on Fetus and Newborn.Controversies concerning vitamin K and the newborn[J].Pediatrics,2003,112:191-192.
[5]Shiqing Songa,Xiaoming Zhanga,Khizar Hayat,et al.Contribution of beef base to aroma characteristics of beeflike process flavour assessed by descriptive sebsory analysis and gas chromatography olfactometry and partial least squares regression[J].Journal of Chromatography A,2010,1217(49):7788-7799.
[6]李向荣.绿色蔬菜中维生素K1的薄层_紫外分光光度法测定[J].中国公共卫生,1996,12(8):246.
[7]赵建国,耿聪,齐懿鸣.乳粉中维生素K1高效液相色谱测定方法的改进[J].分析测试技术与仪器,2005,11(4):311-313.
[8]聂西度.高效液相色谱法测定谷物中维生素Kl的含量[J].食品研究与开发,2005,26(4):130-131.
[9]谭建华,席绍峰.高效液相色谱法测定化妆品中的维生素K1[J].分析测试学报.2012,31(11):1451-1454.
[10]邓峰,周英田.高效液相色谱法对食品中维生素K1的定量测定[J].色谱,1996,14(3):233-234.
[11]郝岩平,刘波.乳品中维生素K1的测定[J].中国乳品工业,2003,31(1):30-31.
[12]铁晓威.高效液相色谱柱后衍生法测定食品中的VK1[J].食品与发酵工业,2002,28(9):34-37.
[13]姜瑞清.对GB 5413.10-2010中维生素K1检测的改进研究.中国乳品工业,2011,39(9):50-52.
[14]GB 5413.10-2010婴幼儿食品和乳品中维生素K1的测定[S].
[15]GB 5009.158-2016食品安全国家标准食品中维生素K1的测定[S].