石榴健胃胶囊中非法添加尼扎替丁、西咪替丁、法莫替丁、盐酸雷尼替丁和拉呋替丁的检测

目的:建立石榴健胃胶囊中非法添加尼扎替丁、西咪替丁、法莫替丁、盐酸雷尼替丁和拉呋替丁的分析方法.方法:采用高效液相色谱法,以十八烷基硅烷键合硅胶为填充剂的C18柱(4.6 mm×250 mm,5 μm),以甲醇(A)-水(每1 000 mL含磷酸0.3 mL和己烷磺酸钠0.94g)(B)梯度洗脱0～25 min,A:23％,B:77％；25～ 40 min,A:23％→90％,B:77％→10％；40 ～ 50min,A:23％,B:77％]；流量为1.0 mL·min -1;柱温小于30 ℃；检测波长为220 nm.结果:尼扎替丁、西咪替丁、法莫替丁、盐酸雷尼替丁和拉呋替丁的线性范围分别为0.020 34 ～2.542 μg(r ＝0.999 9)、0.020 78～2 598 μg(r＝0.999 9)、0.018 86～2.357 μg(r＝0.999 9)、0.019 66～2.457 μg(r＝1)和0.022 06 ～ 2.757 μg(r ＝0.999 9)；回收率(n＝6)分别为101.53％、94.09％、92.24％、93.44％和96.38％；RSD分别为0.81％、0.53％、0.49％、0.90％和0.92％.结论:该方法选择性强,灵敏度高,重复性好,亦可作为石榴健胃胶囊预防非法添加尼扎替丁、西咪替丁、法莫替丁、盐酸雷尼替丁和拉呋替丁的有效分析方法.

Determination of Nizatidine, Cimetidine, Famotidine, Ranitidine Hydrochloride and Lafutidine illegally mixed into ShiliuJianwei Capsules

Objective： To establish an HPLC method for determination of Nizatidine, Cimetidine, Famotidine, Ranitidine Hydrochloride and Lafutidine illegally added into ShiliuJianwei Capsules. Methods： An HPLC method was estabilisbed . C18 （4. 6 mm × 250 mm,5μm） column was used, methanol as mobile phase A, water（ Every 1 000 mL contain phosphate 0. 3 mL and sodium hexanesulfonate 0. 94 g） as mobile phase B ,gradient elution 0 - 25 min, A：23% , B：77% ;25 - 40 min, A： 23% →90% , B ：77%→10% ;40 - 50 rain,A：23% ,B：77% ]. The flow rate was 1 mL · min-1 and the column temperature was before 30 ℃ ,the detection wavelength was 220 nm. Results： The linear ranges for Nizatidine, Cimetidine, Famotidine, Ranitidine Hydrochloride and Lafutidine were 0. 020 34 - 2. 542 μg（ r = 0. 999 9 ） ,0. 020 78 μg -2. 598 μg（ r = 0. 999 9） ,0. 018 86 μg -2. 357 μg（ r = 0. 999 9 ） ,0. 019 66 μg -2. 457 （ r = 1 ） and O. 02206μg-2. 757μg（ r = 0. 9999 ）. The average recovery of Nizatidine, Cimetidine, Famotidine, Ranitidine Hydrochloride and Lafutidine was 101.53% ,94. 09% ,92. 24% ,93.44% and 96. 38% （ n = 6） with RSD of 0. 81% ,0. 53% ,0. 49% ,0. 90% and 0. 92% respectively. Conclusion： The method is specific, sensitive, repetitive and accurate, thus it can be used to determination of Nizatidine, Cimetidine , Famotidine, Ranitidine Hydrochloride and Lafutidine which were illegally added to ShiliuJianwei Capsules.