摘要
提出了高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定不同基质调节尿酸类功能性食品中21种性质差异较大的急慢性痛风药物含量的方法。样品按照主要基质成分分类(植物类、活性肽类、油脂类),采用不同的前处理优化方法,再进一步优化仪器工作条件。采用ACQUITY UPLC BEH C_(18)色谱柱对21种药物进行分离,含5 mmol·L^(-1)甲酸铵的0.1%(体积分数)甲酸溶液-乙腈作为流动相进行梯度洗脱,电喷雾离子源正负离子模式同时扫描,多反应监测模式检测,外标法定量。结果表明,21种药物的质量浓度在一定范围内与对应的峰面积呈线性关系,检出限(3S/N)为0.03~0.25μg·kg^(-1)。按照标准加入法进行回收试验,回收率为63.6%~118%,测定值的相对标准偏差(n=6)均小于10%。在实际样品检测过程中,可采用同一种代表性空白样品溶液制作通用型的基质匹配标准曲线消除基质效应,可有效降低试验成本,节约时间。方法应用于50批样品的检测,其中2批样品检出别嘌醇。
In regulating uric acid fuctional food with different matrices,a method for simultaneous determination of 21 acute and chronic gout drugs,possessing various physicochemical properties,by high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)was proposed.The samples were classified according to the main substrate composition(plants,active peptides,oil),and then the pretreatment and instrument analysis were optimized.21 drugs were separated on ACQUITY UPLC BEH C_(18)column,using 0.1%(volume fraction)formic acid containing 5 mmol·L^(-1)ammonium formate-acetonitrile as the mobile phase for gradient elution,and then analyzed under the multiple reaction monitoring mode with positive or negative ion mode by electric spray ion source.External standard method was used for quantitative analysis.As shown by the results,linear relationships between values of the corresponding peak area and mass concentration of 21 drugs were found in definite ranges,with detection limits(3S/N)in the range of 0.03-0.25μg·kg^(-1).Test of recovery was made by the standard addition method,giving results in the range of 63.6%-118%,with RSDs(n=6)of the determined values less than 10%.The general matrix matching standard curves could be prepared by using the same representative blank sample solution to eliminate the matrix effect,which could effectively reduce the experimental cost and save time.This method was applied to the detection of 50 batches of samples,and allopurinol was detected in 2 batches of samples.
作者
綦艳
邓幸飞
许庆鹏
杨俊业
吴思敏
李聪
QI Yan;DENG Xingfei;XU Qingpeng;YANG Junye;WU Simin;LI Cong(Guangdong Testing Institute of Product Quality Supervision,Foshan 528300,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2023年第3期274-282,共9页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
广州市科技计划项目(202102080652)
国家市场监督管理总局科技计划项目(2020MK080)。
作者简介
綦艳,高级工程师,硕士,研究方向为食品及食品相关产品检测与方法开发;通讯联系人:邓幸飞,329520539@qq.com。
