纳米银表面增强拉曼光谱法测定保健食品中非法添加的4种地平类降压药物

应用表面增强拉曼光谱法(SERS)测定了保健食品中非法添加的4种属于二氢吡啶类的降压药物,即盐酸贝尼地平(BNDP)、盐酸尼卡地平(NCDP)、硝苯地平(NFDP)和阿雷地平(ADP)。称取经碾碎的疑似添加降压药物的保健食品0.1030g,用甲醇10.0mL超声提取5min,离心后取其上清液1.0mL,加入甲醇定容至10.0mL。分取此溶液100μL,加入纳米银溶液200μL作为表面增强剂及体积比为2∶7的盐酸溶液20μL作为助剂,用振荡器以400r·min^-1的转速振荡10s,按仪器工作条件进行SERS测定。测得BNDP和NCDP的质量浓度在1.0~10.0mg·L^-1内分别与两者对应的特征峰比值呈线性关系;NFDP的线性范围为2.0~9.0mg·L^-1,ADP的线性范围为1.0~9.0mg·L^-1。它们的检出限(3S/N)依次为0.40,0.45,0.75,0.75mg·L^-1。按标准加入法进行回收试验,测得ADP的回收率为96.0%,其他3种药物的回收率为108%。各测定值的相对标准偏差(n=5)为1.0%~5.9%。按本方法分析了一件缴获的样品,测得其中含NCDP为10.4%。

Determination of Four Diping Anti-Hypertensive Drugs Illegally Added in Healthcare Foodstuffs by Nano-Silver Surface Enhanced Raman Spectroscopy

Surface enhanced Raman spectroscopy(SERS)was applied to the determination of illegally added anti-hypertensive drugs4of which were chosen to be studied in this work,namely benidipine hydrochloride(BNDP),nicardipin hydrochloride(NCDP),nifedipine(NFDP)and adipine(ADP)]in health-care foodstuffs.As shown by their molecular structures,these 4drugs were classified to dihydropyridines.A portion(0.1030g)of the crushed sample,suspected for adding the contraband drugs,was ultra-sonicated for 5min with 10.0mL of methanol to extract the drugs into the solvent.After centrifugation,1.0mL of the supernatant was taken and made its volume to 10.0mL with methanol.An aliquot of 100μL of the solution was taken and 200μL of the nano-silver solution(as surface enhancer)together with 20μL of hydrochloric acid solution with a volume ratio of 2∶7(as auxiliary)were added.After shaking for 10sat a rotation rate of 400r·min^-1,the solution was ready for SERS determination under the prescribed working condition of the instrument.Linear relationships between values of intensity ratios of the characteristic peaks found and relative mass concentrations of the 4drugs were found in the following ranges:①from 1.0-10.0mg·L^-1,same for DNDP and NCDP;②from 2.0-9.0mg·L^-1 for NFDP;and③from 1.0-9.0mg·L^-1 for ADP.Values of detection limits(3S/N)found of the 4drugs were 0.40,0.45,0.75,0.75mg·L^-1 respectively.Recovery was tested by standard addition method,giving results of recovery of 96%for ADP,and at same value of 108%for the remainder 3drugs.Values of RSDs(n=5)found were ranged between 1.0%and 5.9%.A seized sample was analyzed by the present method,NCDP was found with its content of 10.4%.