| Macroporous absorbing resins were used widely in extraction components of traditional Chinese drug and Chinese patent medicine in recent ten years. But there have had no complete and formal technique standards now. A GC method using wide bore open tubular columns was established to detect seven residual solvents (benzene, toluene , xylene, styrene , diethylbenzene, divinybengene, decane) in polystyrene-type macroporous absorbing resins. Benzene and toluene was extracted by ultrasound using DMSO. xylene, styrene, diethylbenzene, divinybengene and decane was extracted by ultrasound using alcohol. HP-5 column (30m X 0.53mm i.d.,2.65μm) was used. The detector was FID. The injector and detector temperatures were maintained at 260℃ . 1 μ l samples were injected to GC splitlessly. (alcohol extractions)The oven temperature was 40℃ (10min) 5℃.min-1 80℃(10min) 35℃.min-1 260℃(5min). The carrier gas was helium flowing at a rate of 23ml.min-1 . (DMSO extractions) The oven temperature was 30℃ (15min) 35℃.min-1 260℃ (15min); The carrier gas was helium flowing at a rate of 14ml.min-1. seven residual solvents respectively had excellent linearity over a range of concentrations(benzene r = 0.9999; toluene r=0.9990; xylene r=0.9990; diethylbenzene r= 0.9994; styrene r = 0.9999; divinybengene r = 0.9999; decane r = 0.9990). Limit of detection of benzene, toluene, divinybengene and decane is 0.50μg.ml-1. Limit of detection of xylene, diethylbenzene and styrene is0.20μg.ml-1 .After the method established, we detected seven residual solvents in ten polystyrene-type macroporous absorbing resins under the different conditions(not through pretreatment, through easy pretreatment, through complicated pretreatment). The results showed that the macroporous absorbing resins must be pretreated before used, and alcohol elution stage isvery important to the elimination of the residual solvents.Then we compared three different standards of pretreatment(not turbid when adding several times water to the alcohol which through resins. UV method, GC method). The results showed that GC method is optimal.The polyvinylchloride(PVC) bags gradually took the place of the glass bottles as the containers of the intravenous solutions. Many foreign scholars paid attention to the problem of di(2-ethylhexyl)phthalate(DEHP) releasing from the PVC bags. But there is not any report in our country. We established a 530 u m capillary gas chromatography method for determination of DEHP in the intravenous solutions in PVC bags with internal standardization(DOP). HP-5 column (30mX 0.53mm i.d.,2.65um) was used. The detector was FID. The oven temperature was maintained at 260 °C. The injector temperature was 280°C. The detector temperature was 300°C. The carrier gas was helium flowing at a rate of 35ml.min''.l ul samples were injected to GC splitlessly.The standard curves of DEHP were linear in the range 6.00 50.00/xg.ml"'. The average recovery was 99.49%. Limit of detection was 1.16/ig.ml"1.We detected DEHP in 5% glucose intravenous solutions in PVC bags, non-PVC bags and glass bottles. The content of DEHP in PVC bags is more than that in non-PVC bags. And we didn't detect any DEHP in glass bottles.Then we did experiments about the factors that influence the releasing of DEHP. The results showed that the releasing degree of DEHP is different in different intravenous solutions. And the solution which contain more components or whose density is more concentrated would refrain the releasing of DEHP. More vibration and longer store time would increase he releasing of DEHP. Though the light and temperature had little influence on the releasing of DEHP.
|
PDF Full Text Request