[Determination of organic residues in macroporous adsorption resins by gas chromatography].
A method has been developed for the simultaneous determination of benzene, toluene, xylene, styrene, decane, diethylbenzene, undecane, divinylbenzene, dodecane and naphthalene residues in macroporous adsorption resins (MARs). The organic residues were extracted from resin samples by ultrasonic extraction with dichloromethane and analyzed by gas chromatography. The chromatographic conditions were as follows: a DB-624 capillary column (30 m x 0.32 mm i.d., 1.8 microm); carrier gas, nitrogen with a flow rate of 2.5 mL/min; column temperature, programmed from 40 degrees C to 200 degrees C at a rate of 14 degrees C /min and kept at 200 degrees C for 1 min; flame ionization detector temperature, 250 degrees C; injector temperature, 220 degrees C; splitless injection, 1 microL. All the 10 organic residues were separated well in 12 min. The recoveries for spiked standards (n = 3) were 73.8% - 107.9%. The relative standard deviations were 1.3% - 4.4%. The limits of detection were 0.007 - 0.03 mg/L. This method is sensitive, accurate and quick. Nine commercial MARs and their pretreated samples were assayed, and the results show that the contents of organic residues varied greatly in two kinds of samples. And the pretreated MARs can be used safely in the production of traditional Chinese medicines.
School of Pharmaceutical Sciences, Peking University Health Science Center, Beijing 100083, China. jiacunqin@tom.com
Cunqin
C
Jia
Yangchun
Y
Li
Pengfei
P
Tu
Hongquan
H
Zhang
D000473:Alkanes / Q000032:analysis; D001554:Benzene / Q000032:analysis; D002849:Chromatography, Gas / Q000295:instrumentation* / Q000379:methods*; D009281:Naphthalenes / Q000032:analysis; D016062:Porosity; D015203:Reproducibility of Results; D012117:Resins, Synthetic / Q000737:chemistry*; D020058:Styrene / Q000032:analysis; D014050:Toluene / Q000032:analysis; D014992:Xylenes / Q000032:analysis
D000473:Alkanes; D009281:Naphthalenes; D012117:Resins, Synthetic; D014992:Xylenes; C007548:n-dodecane; C031721:naphthalene; D014050:Toluene; D020058:Styrene; D001554:Benzene; C022884:undecane; C012867:decane