保健食品中盐酸硫胺素、盐酸吡哆醇、烟酸、烟酰胺和咖啡因的测定 编制说明

《保健食品中硫胺素、核黄素、吡哆醇、烟酸、烟酰胺和咖啡因的测定》（征求意见稿）编制说明一、工作简况根据《国家标准化管理委员会关于下达2023年第二批推荐性国家标准计划及相关标准外文版计划的通知》（国标委发〔2023〕372023年11月，全国特殊食品标准化技术委员会秘书处在北京召开《14项保健食品分析方法标准启动会》修订工作启动会，会上二、国家标准编制原则、主要内容及其确定依据本标准是根据GB/T1.1-2020《标准化工作导则第1部分：标素B2的测定》增加了98±2℃水浴加热30min，因组分不加热加热企业自测值（加热）理论投料量核黄素（mg/片）0.712.252.172.22烟酰胺（mg/片）7.547.477.497.50吡哆醇（mg/片）2.312.342.172.25硫胺素（mg/片）2.212.292.152.25对于磷酸酯形式的维生素，样品经取样后，加入10mg酸性磷高，并处于标示范围内。经验证，在pH=4.5时酶的活力较pH=2.0（加热）-0.1%磷酸（pH2.0)-0.1%磷酸（pH4.5)盐钠盐通过采用二极管阵列检测器考察了6种目标物的紫外吸收光谱图。结果显示硫胺素、核黄素、烟酸、烟酰胺在260n动相中磷酸浓度为0.1%时，烟酸色谱峰明显前沿，将磷酸浓度提高三、试验验证的分析、综述报告在97.0%～104.6%，相对标准偏差RSD在0.2%～3.2%；核黄素的三种浓度加标回收率在94.7%～102.9%，相对标准偏差RSD在0.2%～2.2%；烟酸的三种浓度加标回收率在99.0%～108.2%，相对标准偏差RSD在0.3%～4.5%；烟酰胺的三种浓度加标回收率在浓度加标回收率在98.5%～107.0%，相对标准偏差RSD在0.2%~3.1%；硫胺素的三种浓度加标回收率在97.3%～108.5%，相对标准四、与国际、国外同类标准技术内容的对比情况五、以国际标准为基础的起草情况六、与有关法律、行政法规及相关标准的关系七、重大分歧意见的处理经过和依据八、涉及专利的有关说明九、实施国家标准的要求，以及组织措施、技术措施、过渡期和实施日期的建议建议本标准发布6个月后实施，由归口单位组织行业相关单位十、其他应当说明的事项附件：方法学验证报告保健食品中硫胺素、核黄素、吡哆醇、烟酸、烟酰胺和咖啡因的测定方法学验证 40 20 40 20 mAU 80 60 40 20 2030 mAU 80 60 40 20 2030 mAU 80 60 40 20 2030 mAU 80 60 40 20 2030 mAU 80 60 40 20 2030 mAU 80 60 40 20 2030 mAU 80 60 40 20 2030 mAU 80 60 40 20 2030mAU806040200咖啡因吡哆醇吡哆醇02030mAU806040200核黄素烟酸烟酰胺硫胺素核黄素烟酸烟酰胺硫胺素02030纯MicroPuliteXPRP18Plus、月旭UltimatePolar-RPC18均能够对六），2.检出限95%时，最终确定检出限1）固体或半固体试样3.定量限本标准选择4种典型空白基质样品：片剂、软胶囊、凝胶糖果、4.测定范围咖啡因浓度(μg/mL）01252050峰面积023.9348.36120.00240.03481.801201.76线性方程Y=24.039590X+0.057849相关系数1.0000核黄素浓度(μg/mL）01252050峰面积039.7579.23200.45399.95799.552012.33线性方程Y=40.242286X-1.438136相关系数1.0000酸烟浓度(μg/mL）01252050峰面积021.0644.66107.87217.58437.291093.48线性方程Y=21.876376X-0.453670相关系数1.0000烟酰胺浓度(μg/mL）01252050峰面积023.3447.00230.46460.01线性方程Y=23.116753X-0.296549相关系数1.0000吡哆醇浓度(μg/mL）01252050峰面积021.3742.13104.48211.25420.261054.97线性方程Y=21.095138X-0.272820相关系数1.0000硫胺素浓度(μg/mL）01252050峰面积022.1545.68230.77465.40线性方程Y=23.385260X-1.44737相关系数1.00005.正确度吡哆醇的加标回收率在101.7～107.0%，相对标准偏差RSD在1.5~吡哆醇的加标回收率在99.2～103.5%，相对标准偏差RSD在0.3~吡哆醇的加标回收率在98.5～103.4%，相对标准偏差RSD在0.2~称123456102.9899.55105.36104.24102.62.198.3595.6194.6694.2297.8595.62.2106.37110.54110.39108.25109.69108.22.4104.45108.71109.44110.742.8105.74108.98107.65107.29107.03.1105.34110.94110.48108.43109.30106.78108.52.0 液体咖啡因102.25104.94101.5299.92100.81101.24101.81.7100.9798.8799.2298.0996.9197.2898.6105.54102.88102.73101.01107.302.2101.7596.61100.6796.95106.74108.70101.94.999.86103.34104.83100.80103.40102.6105.34100.8199.92100.52100.76101.496.2596.4798.2095.6699.2898.33.296.4292.9993.3896.8295.094.73109.06103.95101.95103.39102.81102.64.5100.29103.03104.75103.6298.62100.71101.82.3103.35105.52104.39101.51104.90103.6103.93103.47103.63104.31104.67103.84104.00.4104.36102.72106.24106.47105.55102.52104.6102.9697.8897.6296.6899.2598.6198.82.2104.52103.07105.02104.28103.74104.28104.20.698.49100.4397.95100.51102.6297.7699.699.5998.79101.61103.35104.05102.74101.72.196.2098.2996.4997.9297.8196.8297.30.912345699.9397.8596.9396.7796.7596.8797.598.6498.2998.3097.7897.7698.2698.20.3102.87104.45104.95104.26104.41104.80104.30.7102.09104.09104.69103.78104.01104.62103.90.9101.77103.33103.48102.98103.47103.500.7100.56103.33103.56102.46103.36102.90102.7101.08101.32101.24100.91100.70100.89101.00.297.9593.9793.8193.3795.2394.7101.33102.54102.25103.35102.60.7101.44100.45104.79103.403.0100.96101.42101.86101.71102.23101.65101.60.4101.48100.40101.37100.98101.37101.00.6102.6195.3696.7197.0495.9294.3097.03.0100.6496.4696.0195.9297.7997.2102.96104.86104.37104.90105.55105.01104.60.9101.84103.57103.74103.80103.74103.02103.30.7103.20103.79103.26103.87103.60103.02103.50.3100.84102.36102.65102.35102.420.6100.8899.88102.0598.02101.9997.77101.9997.7797.9199.64102.0797.69100.21101.998.299.70.50.598.8498.9398.0198.6899.0198.60.499.5199.0399.7698.9399.2698.7499.20.498.9198.9199.0998.7099.00.2123456101.86102.04101.90101.90102.01101.80.3102.08102.82103.08102.90.4101.99102.22101.96102.09102.03101.90.4100.70101.78101.88102.08102.04102.27101.80.5101.37101.95102.26102.28102.32102.250.4101.05101.85101.98102.01101.70101.66101.70.398.5299.9699.9799.90100.0899.80.699.3299.9899.7199.8899.9599.8799.80.298.3299.2798.3299.3599.4899.00.595.5898.0097.6697.8497.7097.9497.598.3098.7798.5598.8998.9298.8398.70.299.0498.8898.9098.6898.9698.80.3103.42101.95101.80101.46102.20.7102.62102.99102.78102.82103.05102.92102.90.2103.89104.77104.73105.09104.77104.54104.60.4100.97101.80101.98101.60101.79101.50.4102.74103.34103.45103.47103.41103.87103.40.4102.74103.67103.57103.55102.66103.20.499.0698.3397.6097.7597.5097.5198.00.6100.4996.8896.7396.5196.4397.498.4599.0999.3499.2599.10.397.3597.5097.4497.3697.3997.4697.40.198.2298.4498.7298.8198.5498.4398.50.298.0798.4798.2998.2197.9697.9898.20.26.标准储备液稳定性单标储备溶液浓度变化无显著性差异，表明六种组分在4℃-8℃冰箱177.再现性（实验间方法验证）编号指标含量（g/100g）RSD(%)Lab1Lab2Lab3Lab4Lab5片剂咖啡因＜0.03<0.03<0.03＜0.03＜0.03/核黄素0.4580.4590.4480.4860.4803.45烟酸＜0.03<0.03<0.03＜0.03＜0.03/烟酰胺4.774.844.864.934.76吡哆醇0.6690.6320.6730.66