液体伤口敷料中非法添加维生素检测方法研究  

Detection Methods for Illegal Addition of Vitamin in Liquid Wound Dressing

作　　者：李煜 陈超 王丹 LI Yu;CHEN Chao;WANG Dan(Zhejiang Institute for Food and Drug Control·Key Laboratory of Drug Contacting Materials Quality Control of Zhejiang Provincial,Hangzhou,Zhejiang,China 310052)

机构地区：[1]浙江省食品药品检验研究院·浙江省药品接触材料质量控制研究重点实验室,浙江杭州310052

出　　处：《中国药业》2024年第21期71-74,共4页China Pharmaceuticals

基　　金：浙江省基础公益研究计划项目[LTGC23H300002]。

摘　　要：目的建立定性定量检测液体伤口敷料中非法添加烟酰胺和维生素B6的高效液相色谱法和液相色谱-质谱法。方法定量方法中,色谱柱为Waters Sunfire C_(18)柱(250 mm×4.6 mm,5μm),流动相为0.1%庚烷磺酸钠溶液(用甲酸调pH至2.5)-甲醇(梯度洗脱),检测波长为261 nm(烟酰胺)和290 nm(维生素B6),经外标法定量。定性方法中,色谱柱为Waters Acquity HSS T3 C_(18)柱(100 mm×2.1 mm,1.8μm),流动相为0.1%甲酸水溶液-甲醇(95∶5,V/V),电喷雾离子化检测,正离子下多反应监测(MRM)模式。结果定量方法中,烟酰胺的质量浓度在0.01~200μg/mL范围内、维生素B6的质量浓度在0.05~100μg/mL范围内与峰面积线性关系良好(r=1.0000,n=5);检测限分别为0.023,0.010μg/mL,定量限分别为0.081,0.042μg/mL;平均加样回收率分别为98.47%~100.63%和99.06%~101.13%,RSD分别为0.23%~1.52%和0.14%~3.36%。2批样品中,烟酰胺的含量为0.30%~0.31%,维生素B6的含量为0.048%~0.050%。定性方法中,烟酰胺和维生素B6的检测限分别为0.5,0.1 ng/mL。结论该方法快速简便、灵敏度高,可用于液体伤口敷料中非法添加烟酰胺和维生素B6的定性和定量检测。Objective To establish a high-performance liquid chromatography and liquid chromatography-mass spectrometry method for the qualitative and quantitative detection of illegal addition of nicotinamide and vitamin B6 in liquid wound dressing.Methods In the quantitative method,the chromatographic column was Waters Sunfire C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was 0.1%sodium heptanesulfonate solution(adjusted to pH 2.5 with formic acid)-methanol(gradient elution),the detection wavelength was set at 261 nm for nicotinamide and 290 nm for vitamin B6,and the quantification was determined by the external standard method.In the qualitative method,the chromatographic column was Waters Acquisition HSS T3 C_(18) column(100 mm×2.1 mm,1.8μm),the mobile phase was 0.1%formic acid aqueous solution-methanol(95∶5,V/V),and electrospray ionization detection was adopted with multi-reaction monitoring(MRM)mode under positive ions.Results In the quantitative method,the linear ranges of nicotinamide and vitamin B6 were 0.01-200μg/mL and 0.05-100μg/mL(r=1.0000,n=5),respectively;the limits of detection(LOD)were 0.023μg/mL and 0.010μg/mL,respectively,and the limits of quantification(LOQ)were 0.081μg/mL and 0.042μg/mL,respectively;the average recoveries of nicotinamide and vitamin B6 were in the ranges of 98.47%-100.63%and 99.06%-101.13%,with RSDs of 0.23%-1.52%and 0.14%-3.36%,respectively.The contents of nicotinamide and vitamin B6 in the two batches of samples were in the ranges of 0.30%-0.31%and 0.048%-0.050%.In the qualitative method,the limits of detection of nicotinamide and vitamin B6 were 0.5 ng/mL and 0.1 ng/mL,respectively.Conclusion This method is fast,simple,and highly sensitive,which can be used for qualitative and quantitative detection of illegal addition of nicotinamide and vitamin B6 in liquid wound dressing.

关 键 词：液体伤口敷料 烟酰胺 维生素B6 非法添加 定性检测 定量检测 

分 类 号：R955[医药卫生—药学]