LI Chang-jiang1a,OU Mei-xian2,WANG Sheng-zi1b*,HUANG Tao-min1c,CHEN Nian-zu1c
a Department of Otorhinolaryngology;b Department of Radiation Oncology;c Department of Pharmacy;1 Eye Ear Nose Throat Hospital of Fudan University,Shanghai 200031,China;2 Central Laboratory,Shanghai Xuhui Central Hospital,Shanghai 200031,China
Abstract��
Objective To establish an HPLC-MS/MS method (high performance liquid chromatography-tandem mass spectrometry) for the direct determination of amifostine in human saliva. METHODS Saliva samples were collected from six adult healthy volunteers. After protein precipitation and addition of the internal standard (IS) huperzine-A (HupA),HPLC- MS/MS was used to analyze amifostine. The analysis was conducted using a ZIC�k-HILIC analytical column (2.1 mm×100 mm,3.5 μm). Electrospray ionization was used with multiple reaction monitoring (MRM) mode. RESULTS The lower limit of quantification (LLOQ) of the method was 0.938 mg·L-1 (S/N>10). The standard curve was linear in the range of 0.938-30 mg·L-1 (r=0.999 1,n=6). The inter-day and intra-day RSDs were all less than 15% for the low,medium and high concentration quality control samples (1.0,5.0 and 25 mg·L-1 ). The values of recovery were all more than 85%. CONCLUSION The method is direct,rapid,simple and sensitive,and suitable for the determination of amifostine in saliva samples.
LI Chang-Jiang-a,
ŷMei-Xian-,
WANG Sheng-Zi-b* etc
.Determination of Amifostine in Human Saliva by HPLC-MS/MS[J] Chinese Pharmaceutical Journal, 2013,V48(6): 482-484
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