HPLC-MS/MS法同时检测红花药材中9种非法染色物
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篇名: HPLC-MS/MS法同时检测红花药材中9种非法染色物
TITLE:
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 mL/min,柱温为30 ℃,进样量为10 μL。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/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);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。
ABSTRACT: 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 ammonium formate-acetonitrile (gradient elution) at the flow rate of 0.2 mL/min. The column temperature was 30 ℃, and the sample size was 10 μL. Mass spectrometry condition: electrospray 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 orangeⅡ, 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.
期刊: 2017年第28卷第27期
作者: 李婷婷,李良,刘莉,曾桢,孔卫东,刘芬,孙茜
AUTHORS: LI Tingting,LI Liang,LIU Li,ZENG Zhen,KONG Weidong,LIU Fen,SUN Qian
关键字: 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
KEYWORDS: HPLC-MS/MS; Carthamus tinctorius; Ponceau; Acid red 73; Lemon yellow; Azorubin; Allura red; Gold orange Ⅱ; Sunset yellow; Pyrosine; Golden orange G
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