Determination of p-Tert-Octylphenol in Medicinal Rubber Stoppers by GC-MS
Objective To establish a gas chromatography-mass spectrometry(GC-MS)method for determining the content of p-tert-octylphenol in medicinal rubber stoppers.Methods The chromatographic column was the Agilent DB-5MS column(30 m x 0.25 mm,0.25 μm),the carrier gas was high-purity helium,the inlet temperature was 250℃,the split ratio was 5∶1,the injection volume was 1 μL,the flow rate was 1.5 mL/min,and the temperature was programed.The ion source temperature was 230℃,the quadrupole temperature was 150℃,the ions at the selective ion monitoring(SIM)mode had a m/z of 57,107,135,136,and the quantitative ion had a m/z of 135(relative abundance of 100％),the solvent cutting time was 4.5 min,and the collection time for the spectrum was 14 min.The p-tert-octylphenol in eight batches of rubber stoppers from three manufacturers was extracted with sodium dihydrogen phosphate buffer(pH 5),ammonia-ammonium chloride buffer(pH 10),50％ethanol,ethanol and dichloromethane,and the external standard method was used for corrected quantification.Results The linear range of p-tert-octylphenol was 0.05-1 μg/mL(r=0.999 9,n=5).The limit of detection was 0.005 μg/mL and the limit of quantification was 0.01 μg/mL.The RSDs of the precision test was lower than 2％,and the recovery rate was in the range of 92.97％to 102.41％,with the RSDs of 6.95％to 14.93％(n=9).The p-tert-octylphenol was detected in six out of eight batches of samples,which was more easily extracted in alkaline and highly-weakly polar organic phase media.Conclusion This method is simple,efficient,sensitive,precise and accurate,which can be used for the determination of p-tert-octylphenol in medicinal rubber stoppers.
gas chromatography-mass spectrometrymedicinal rubber stopperp-tert-octylphenolcontent determination
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