Determination of ethylene chlorohydrin, ethylene dibromide and other volatile fumigant residues in flour and whole wheat.
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Isothermal gas chromatography with flame ionization detection was used to determine residual ethylene oxide (EtO), ethylene chlorohydrin, and ethylene glycol in soft rubber catheters that had been sterilized with EtO. Catheter samples were extracted by shaking with carbon disulfide, and the extract was analyzed on a 3% Carbowax 20M on 80-100 mesh Chromosorb 101 column, using nitrogen as the carrier gas. Ten replicate injections of a mixed standards solution gave coefficients of variation of 1.91, 1.23, and 4.74% for EtO, ethylene chlorohydrin, and ethylene glycol, respectively. A linear response was obtained with concentrations ranging from 1.0 to 7.9 micrograms EtO, 14.0 to 88.0 micrograms ethylene chlorohydrin, and 31.0 to 98.5 micrograms ethylene glycol. The proposed method detected as little as 0.5, 5.0, and 16.5 ng EtO, ethylene chlorohydrin, and ethylene glycol, respectively.
Ethylene chlorohydrin (2-chlorethanol) and ethylene glycol can originate as by-products during ethylene oxide sterilization. We studied the effect of these subsdtances upon human HeLa cells as well as the conjunctiva and the epithelium of the external genitalia of 35 rabbits. - We found ethylene chlorohydrin to be considerably more toxic than ethylene glycol. 2-chloroethanol did not cause any reactions at our cell cultures in dilutions of 1:100 after 4 h action upon the cells and 24 h observation time. In our experimental animals this concentration had only minimal irritating effects at the external genitalia. Ethylene glycol produced cellular damages in dilutions of 1:10 after 5 d only. Our experimental animals showed no reactions to these concentrations. At the conjunctiva of rabbits dilutions of 1:100 ethylene chlorohydrin and 1:10 ethylene glycol had no effect. After application of 2-chloroethanol 1:100 to the external genitalia minimal irritations were observed. Ethylene glycol in dilutions of 1:5 caused irritations of the conjunctiva and the genitalia of our rabbits. Ethylene chlorohydrin- and ethylene glycol concentrations which had a damaging effect upon our cell cultures of our experimental animals were many times higher than those which might be expected to originate during ethylene oxide sterilization.
A gas chromatographic procedure is described for the quantitative determinations of ethylene chlorohydrin and ethylene glycol in disposable medical-grade plastics. Both components are isolated by solvent extraction. The lower limit of detection is 1 p.p.m. of ethylene chlorohydrin and 2 p.p.m. of ethylene glycol. Propylene glycol is used as an internal standard. Ethylene oxide residues have to be removed prior to the assay.
A gas chromatographic (GC) method was developed for the determination of ethylene oxide and its two reaction products, ethylene chlorohydrin and ethylene glycol, in aqueous ophthalmic solutions. Propylene oxide was used as an internal standard. All three components were determined in one isothermal chromatographic analysis in less than 15 min. An extraction method for the determination of ethylene oxide residues in plastic components was also developed, and certain plastics with different ethylene oxide retention characteristics were identified.
A GLC method was developed for the determination of ethylene oxide and its two reaction products, ethylene chlorohydrin and ethylene glycol, in ophthalmic solutions at the levels recently proposed by the Food and Drug Administration. The method requires no extractions, sample preparations, or elaborate trapping and concentrating techniques. All three components can be chromatographed on the same spiral glass column packed with a porous polymer absorbent.
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A convenient rapid gas-chromatographic method is described for the quantitative determination of ethylene chlorohydrin. The method reported herein extracts the ethylene chlorohydrin with water. The method is simple and offers advantages since no elaborate and expensive gas extraction apparatus is required. The ethylene chlorohydrin levels in five different sterilized polyvinyl chloride samples were found to vary between 5 and 25 ppm. The effect of resterilization with ethylene oxide was investigated and was found to produce less ethylene chlorohydrin.
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Published reports on the formation of ethylene chlorohydrin in ethylene oxide-sterilized poly(vinyl chloride) are contradictory. The present paper discusses parameters involved in the ethylene chlorohydrin formation, such as the stabilizer system, plasticizer content and thermal strain during manufacture. It is shown that ethylene chlorohydrin can be formed in ethylene oxide-sterilized poly(vinyl chloride) previously sterilized by irradiation, in amounts dramatically exceeding published 'safe levels'.
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A simultaneous determination of ethylene glycol (EG) and ethylene chlorohydrin (EC), which are formed during sterilization of bone and dura mater with ethylene oxide, has been reported. The EG and EC residues in tissues were extracted with HPLC grade water and analyzed by reversed-phase high-performance liquid chromatography (HPLC) with a RefractoMonitor detector. The isocratic elution was employed with HPLC grade water as the solvent. Since the reference chamber of the detector was filled with solvent and was not changed during the run, the use of gradient programming was not employed. With spherisorb ODS (5 microns) C18 column and 20 microL sample injection, the retention times for EG and EC were (104 +/- 2) sec and (202 +/- 4) sec, respectively. The unknown concentration was calculated from the calibration curve and the weight of the sample tissue. The HPLC analysis provided a simple, accurate and reproducible method of determination of EG and EC residues in ethylene-oxide sterilized tissues.
We have previously described a very sensitive and efficient bacterial test designed to detect chemical carcinogens as mutagens. Chloroacetaldehyde is mutagenic in this system and is of interest because it is a possible metabolite in mammals of the large volume industrial chemicals 1,2-dichloroethane (ethylene dichloride) (3.5 billion kg/yr, U.S.) and vinyl chloride (2.5 billion kg/yr, U.S.), and of the antineoplastic agent cyclophosphamide. Chloroacetaldehyde reverts a new Salmonella bacterial tester strain (TA100). Chloroacetaldehyde is shown to be hundreds of times more effective in reversion of TA100 than is chloroethanol (ethylene chlorohydrin), a known metabolic precursor of chloroacetaldehyde and a possible metabolite of dichloroethane and vinyl chloride, or than vinyl chloride, which is itself mutagenic for TA100. Chloroethanol is shown to be activated by rat (or human) liver homogenates to a more highly mutagenic form with reversion properties similar to chloroacetaldehyde. Reversion properties of cyclophosphamide after in vitro metabolic activation suggest that chloroacetaldehyde is not the active mutagenic form of this antineoplastic drug.