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1Simultaneous and interference-free determination of eleven nonsteroidal anti-inflammatory drugs illegally added into Chinese patent drugs using chemometrics-assisted HPLC-DAD strategy显示文摘In this work, a smart strategy that combines three-way high performance liquid chromatography-diode array detection(HPLCDAD) data with second-order calibration method based on alternating trilinear decomposition(ATLD) algorithm was proposed for simultaneous determination of eleven non-steroidal anti-inflammatory drugs(NSAIDs) illegally added into Chinese patent drugs and health products. All target analytes were rapidly eluted out within 14.5 min under a simple gradient elution. With the aid of the prominent 'second-order advantage' of the ATLD algorithm, three HPLC problems, i.e. peak overlaps, unknown interferences and baseline drift, could be mathematically calibrated, and pure signals of target analytes could be extracted out from heavy-interference but information-rich HPLC-DAD data. The average spiked recoveries for all target analytes were in the range of 95.9%–106.4% with standard deviations lower than 7.5%. Validation parameters including sensitivity(SEN), selectivity(SEL), limit of detection(LOD), limit of quantitation(LOQ) and precisions of intra-day and inter-day were calculated to validate the accuracy of the proposed method, quantitative results were further confirmed by the classic HPLC method, which proved that chemometrics-assisted HPLC-DAD analytical strategy was highly efficient, accurate and green for drug-abuse monitoring of NSAIDs in Chinese patent drugs and health products.Tong Wang Hai-Long Wu Li-Xia Xie Zhi Liu Wan-Jun Long Li Cheng Yu-Jie Ding Ru-Qin Yu 2018Science China Chemistry2018,61,6:2
2分子荧光结合多维校正测定小龙虾中氨基脲残留量显示文摘近年来,食品中的抗生素残留是人们关心的食品安全问题之一。为测定小龙虾中氨基脲残留量(SEM),本文提出一种基于三维荧光结合化学计量学测定小龙虾中SEM残留量的方法。样本经过简单的前处理,使用2-羟基-1-萘甲醛(2-HN)与SEM进行衍生化反应,生成具有荧光性质的2-羟基萘醛呋喃西林代谢衍生物(SEM-HN)。采集样本的荧光光谱,获得三维荧光数据矩阵;扣除空白样,采用平行因子分析(PARAFAC)算法和交替三线性分解算法(ATLD)对三维荧光数据矩阵进行分析,两种算法均能得到较好的定量分析结果。为了评估两种算法的准确性,对品质因子:灵敏度(SEN)、选择性(SEL)、检出限(LOD)和预测均方根误差(RMSEP)进行计算,结果表明两种算法准确性较好。为进一步验证PARAFAC算法和ATLD算法的性能,采用椭圆置信区间(EJCR)检验,结果本试验中ATLD算法优于PARAFAC算法。结论:三维荧光结合ATLD算法可快速测定小龙虾中的SEM残留。雷渊雄 夏阿林 黄炜 侯泰东 2023中国食品学报2023,23,3:1
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