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

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

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,5μm),以甲醇(A)-水(每1 000 mL含磷酸0.3 mL和己烷磺酸钠0.94 g)(B)梯度洗脱[0～25 min,A:23%,B:77%;25～40 min,A:23%→90%,B:77%→10%;40～50 min,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 34～2.542μg(r=0.999 9)、0.020 78～2.598μg(r=0.999 9)、0.018 86～2.357μg(r=0.999 9)、0.019 66～2.457μg(r=1)和0.022 06～2.757μg(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。

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.