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复合固相萃取净化-液相色谱法测定奶粉中的维生素D

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建立婴幼儿配方奶粉中维生素D的复合固相萃取净化-液相色谱检测方法.样品经石油醚提取,复合固相萃取柱净化,C18色谱柱(250 mm×4.6 mm,5 μm)分离,采用液相色谱-紫外检测器进行测定,外标法定量.维生素D2和维生素D3在0.040,0.100,0.200,0.500,1.000和3.000 mg/L范围内线性关系良好,相关系数为0.999 5和0.999 6,方法定量限为0.015 mg/kg,方法检出限为0.005 0 mg/kg.在0.015,0.050和0.75 mg/kg这3个质量分数水平下回收率在80.7%~98.5%之间,相对标准偏差(SRSD,n=6)在2.51%~7.93%之间.该方法操作简单、准确,具有较高的灵敏度,适合婴幼儿配方奶粉中维生素D含量的测定.
Determination of Vitamin D in Infant Formula Milk Powder by Composite Solid Phase Extraction Purification and Liquid Chromatography
A method using liquid chromatography was developed for the determination of vitamin D in infant formula milk powder.The sample was extracted with petroleum ether followed by clean-up with composite solid phase cartridge.The liquid chromatography separation was performed on C18 column(250 mm×4.6 mm,5 μm).It was determined by liquid chromatography-ultraviolet detector and quantified by external standard method.The calibration curves of vitamin D2 and vitamin D3 showed a good linearity in the range of 0.040,0.100,0.200,0.500,1.000 and 3.000 mg/L,and the correlation coefficients were 0.999 5 and 0.999 6.The limits of detection of vitamin D2 and vitamin D3 were 0.005 0 mg/kg.The limits of quantification were 0.015 mg/kg.The recoveries of milk powder spiked at 0.015,0.050 and 0.75 mg/kg were 80.7%-98.5%,and the relative standard deviations(SRSD,n=6)were 2.51%-7.93%.The method was simple,accurate and sensitive,and could effectively meet the quantitative determination of vitamin D in infant formula milk powder.

liquid chromatographyvitamin Dmilk powdercomposite solid phase extraction purification

杨明、邢丽丽、章路、沈雄雅、葛磊、孙文闪

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杭州郝姆斯食品有限公司(杭州 310000)

绿城农科检测技术有限公司(杭州 310000)

液相色谱 维生素D 奶粉 复合固相萃取

2021年杭州市科技计划引导项目(农业与社会发展)

2021123IY112

2024

食品工业
上海市食品工业研究所

食品工业

影响因子:0.47
ISSN:1004-471X
年,卷(期):2024.45(4)
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