HPLC-MS/MS法同时检测红花药材中9种非法染色物  

Simultaneous Determination of 9 Illegal Dyes in Carthamus tinctorius by HPLC-MS/MS

作　　者：李婷婷 李良[2] 刘莉 曾桢 孔卫东 刘芬[3] 孙茜 

机构地区：[1]成都市食品药品检验研究院,成都610045 [2]武警江西总队医院,南昌330006 [3]南昌大学药学院,南昌330031 [4]上海市宝山区仁和医院,上海200431

出　　处：《中国药房》2017年第27期3842-3845,共4页China Pharmacy

基　　金：江西省卫生计生委中医药科研课题(No.2015A069)

摘　　要：目的:建立同时检测红花药材中9种非法染色物的方法。方法:采用高效液相色谱-串联质谱法(HPLC-MS/MS)。色谱条件:色谱柱为SB-C18,流动相为10 mmol/L甲酸铵-乙腈(梯度洗脱),流速为0.2 m L/min,柱温为30℃,进样量为10μL。质谱条件:离子源为电喷雾离子源,监测方式为负离子多离子反应监测,离子喷雾电压为3 500 V,干燥气温度为350℃,干燥气流速为10 L/min,碰撞气为高纯氮气,扫描范围为m/z 50~1 000。结果:丽春红、酸性红73、柠檬黄、偶氮玉红、诱惑红、金橙Ⅱ、日落黄、赤藓红和金橙G检测质量浓度线性范围分别为5.313 5~531.35 ng/m L(r=0.987 0)、1.312 0~1 312.00 ng/m L(r=0.994 8)、124.4800~2 824.00 ng/m L(r=0.983 2)、6.300 0~630.00 ng/m L(r=0.964 8)、1.035 8~517.92 ng/m L(r=0.996 4)、0.552 0~1 104.00 ng/m L(r=0.909 0)、5.046 3~2 018.52 ng/m L(r=0.996 2)、5.046 3~2 018.52 ng/m L(r=0.997 6)、1.079 5~2 159.00 ng/m L(r=0.9900);定量限分别为10.418 7、1.131 0、68.401 0、13.695 7、1.670 7、0.238 0、3.973 3、1.064 7、1.285 0 ng/kg,检测限分别为3.125 6、0.339 3、20.520 3、4.108 7、0.501 2、0.071 4、1.192 0、0.319 4、0.385 5 ng/kg;精密度、稳定性、重复性试验的RSD<3.0%;回收率为91.2%~99.1%(RSD为0.7%~2.2%,n=6)。结论:该方法专属性强、灵敏度高、简便快捷,适用于红花药材中9种非法染色物的同时检测。OBJECTIVE： To establish the method for the determination of 9 illegal dyes in Carthamus tinctorius. METHODS ： HPLC-MS/MS was adopted. The determination was performed on SB-C18, column with mobile phase consisted of 10 mmol/L ammo- nium formate-acetonitrile （gradient elution） at the flow rate of 0.2 mL/min. The column temperature was 30 ℃, and the sample size was 10 IxL. Mass spectrometry condition： eleetrospray ion source, negative ion multi-ion reaction monitoring mode, ion spray voltage of 3 500 V, drying gas temperature of 350 ℃, drying gas flow rate of 10 L/min, colliding gas of high pure nitrogen gas, scanning range of m/z 50-1 000. RESULTS： The linear ranges of ponceau, acid red 73, lemon yellow, azorubin, allura red, gold orange II , sunset yellow, pyrosine and golden orange G were 5.313 5-531.35 ng/mL（r=0.987 0）, 1.312 0-1 312.00 ng/mL（r= 0.994 8）, 124.480 0-2 824.00 ng/mL（r=0.983 2）,6.300 0-630.00 ng/mL（r=0.964 8）, 1.035 8-517.92 ng/mL（r=0.996 4）, 0.552 0-1 104.00 ng/mL（r=0.909 0）,5.046 3-2 018.52 ng/mL（r=0.996 2）,5.046 3-2 018.52 ng/mL（r=0.997 6）, 1.079 5-2 159.00 ng/mL（r：0.990 0）, respectively. The limits of quantitation were 10.418 7,1.131 0,68.401 0, 13.695 7, 1.670 7,0.238 0, 3.973 3,1.064 7, 1.285 0 ng/kg. The limits of detection were 3.125 6,0.339 3,20.520 3,4.108 7,0.501 2,0.071 4, 1.192 0,0.319 4, 0.385 5 ng/kg, respectively. RSDs of precision, stability and reproducibility tests were all lower than 3.0%. The recoveries were 91.2 % -99.1% （RSD： 0.7 % -2.2 %, n = 6）. CONCLUSIONS： The established method is specific, sensitive, simple and rapid, and can be used for the detection of 9 illegal dyes in C. tinctorius.

关 键 词：高效液相色谱-串联质谱法 红花 丽春红 酸性红73 柠檬黄 偶氮玉红 诱惑红 金橙Ⅱ 日落黄 赤藓红 金橙G 

分 类 号：R927[医药卫生—药学]