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.
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
Keywords
HPLC-MS/MSCarthamus tinctoriusPonceauAcid red 73Lemon yellowAzorubinAllura redGold orange ⅡSunset yellowPyrosineGolden orange G