Microwave-assisted extraction and determination of dicyandiamide residue in infant formula samples by liquid chromatography-tandem mass spectrometry.
A simple, precise, accurate, and validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of dicyandiamide residue in infant formula samples. Following microwave-assisted extraction with 5% formic acid and clean-up on a Sep-Pak AC-2 SPE cartridge, samples were separated on a ZIC-HILIC HPLC column (150 × 2.1mm i.d., 5-µm film thickness; Merck KGaA, Darmstadt, Germany) with 20mM ammonium acetate solution-acetonitrile as mobile phase at a flow rate of 0.25 mL/min. A linear calibration curve was obtained in the concentration range from 1.0 to 50 ng/mL. Infant formula samples were fortified with dicyandiamide at 3 levels, producing average recovery yields of 83.6 to 95.7%. The limits of detection and quantification of dicyandiamide were 3 and 10 μg/kg, respectively. Due to its simplicity and accuracy, the straightforward method is particularly suitable for routine dicyandiamide detection.
College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou 325035, China. Electronic address: shenyan@wzu.edu.cn.
Yan
Y
Shen
Wenzhou Entry-Exit Inspection and Quarantine Bureau of P.R.C, Wenzhou 325027, China.
Chao
C
Han
Zhoushan Entry-Exit Inspection and Quarantine Bureau of P.R.C, Wenzhou 325027, China.
Xiujin
X
Zhou
Wenzhou Entry-Exit Inspection and Quarantine Bureau of P.R.C, Wenzhou 325027, China.
Xiangzhun
X
Chen
Wenzhou Entry-Exit Inspection and Quarantine Bureau of P.R.C, Wenzhou 325027, China.
Fuzhen
F
Huang
Wenzhou Entry-Exit Inspection and Quarantine Bureau of P.R.C, Wenzhou 325027, China.
Zhenou
Z
Zhu
D000818:Animals; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis / Q000302:isolation & purification*; D005506:Food Contamination / Q000032:analysis*; D006146:Guanidines / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D006801:Humans; D007223:Infant; D041943:Infant Formula / Q000737:chemistry*; D008872:Microwaves; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry / Q000379:methods*
D006146:Guanidines; C004711:dicyandiamido
dicyandiamide; infant formula; liquid chromatography-tandem mass spectrometry; microwave-assisted solvent extraction