1.Research on Residues of 16 Phthalate Ester Plasticizers in Oral Liquid Preparations
Hao ZHONG ; Dezhou GE ; Hao LIU ; Zulei DENG
China Pharmacist 2014;(4):556-560
Objective:To establish a GC-MS method for the simultaneous determination of 16 phthalate ester plasticizers in oral liquid preparations, compare the purification effect of liquid preparations by liquid-liquid extraction and solid phase extraction and opti-mize the operating parameters to determine the optimal experimental conditions. Methods:The samples were operated by liquid-liquid extraction and solid phase extraction, respectively. Selective ion monitor ( SIM) was adopt, phthalate esters were identified by the rela-tive abundance of major characteristic ions and the content was determined by an external standard method. Results:When the samples were operated by liquid-liquid extraction, the interference was strong with many impurity peaks. Therefore, the solid phase extraction was adopted for the sample pretreatment. GC-MS was used to detect the residues of 16 phthalate ester plasticizers in oral liquid prepara-tions. The detection limit was 0. 02μg·g-1 ,while the calibration curve showed good linearity within the range of 0. 25-8. 0μg·ml-1 with the correlation coefficient between 0. 990 7 and 0. 999 8. The average recoveries were 76. 0%-95. 4%. The relative standard devi-ations were between 2. 3% and 9. 6%(n=6). Conclusion: Pretreated by solid phase extraction, the residues of 16 phthalate ester plasticizers in oral liquid preparations can be detected by GC-MS with the properties of simple, fast, precise and sensitive, and it is suitable for the determination of phthalate esters in oral liquid preparations.
2.Simultaneous Determination of Three Flavonoids in Tianjihuang Granules by HPLC
Dan ZHAO ; Zulei DENG ; Dezhou GE ; Hao LIU
China Pharmacist 2016;19(7):1415-1417
Objective: To establish an HPLC method for the simultaneous determination of three flavonoids in Tianjihuang gran -ules.Methods:A ZORBAX Eclipse XDB-C18 column was used.The mobile phase was methanol-0.2%phosphoric acid solution (42∶58).The detection wavelength was 350 nm and the flow rate was 1.0 ml· min-1.Results:The linear range of isoquercitrin, quer-citrin and quercetin was 4.572-114.300 μg· ml-1(r=0.999 8), 7.028-175.700 μg· ml-1(r=0.999 8) and 2.195-54.880 μg· ml-1(r=0.999 9), respectively.The average recovery was 98.01%(RSD=1.24%, n=6), 98.14%(RSD=0.98%, n=6) and 97.00%(RSD=1.09%, n=6) , respectively.Conclusion:The method is specific and simple,which can be used for the quality con-trol of Tianjihuang granules.