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    高效液相色谱法同时测定医用敷料类医疗器械产品中17种对羟基苯甲酸酯类化合物的含量

    Simultaneous Determination of 17 Hydroxybenzoate Compounds in Medical Dressing Category Medical Device Products by High Performance Liquid Chromatography

    • 摘要: 在医用敷料类医疗器械产品(样品)中加入体积比8∶2的甲醇-乙腈混合溶液提取后,涡旋混匀,超声提取,离心分离,上清液过0.22 μm滤膜,滤液进入高效液相色谱仪,对羟基苯甲酸酯类化合物(PBs)在ShimNex CS C18色谱柱上用不同体积比的乙腈-0.12%(体积分数)磷酸溶液的混合溶液梯度洗脱分离,外标法定量。结果显示,17种PBs的质量浓度在1~50 mg·L−1内和峰面积呈线性关系,检出限(3S/N)为5~18 mg·kg−1;按照标准加入法进行回收试验,回收率为97.6%~108%,测定值的相对标准偏差(n=6)为0.30%~4.4%;利用该方法筛查10批不同基质的实际样品,PBs检出率为40%,检出对羟基苯甲酸甲酯的样品有1批、对羟基苯甲酸乙酯和对羟基苯甲酸丙酯的样品有3批。

       

      Abstract: After adding the mixed solution of methanol and acetonitrile at volume ratio of 8∶2 into samples of medical dressing category medical device products, vortex mixing, ultrasonic extraction, and centrifugal separation were performed. The supernatant was passed through a 0.22 μm filter membrane, and the filtrate was introduced into the high performance liquid chromatograph. Hydroxybenzoate compounds (PBs) were separated by gradient elution with mixed solutions of acetonitrile and 0.12% (volume fraction) phosphoric acid solution at different volume ratios on the ShimNex CS C18 column, and quantified by the external standard method. It was shown that linear relationships between values of mass concentration and peak area of 17 PBs were kept in the range of 1-50 mg·L−1, with detection limits (3S/N) in the range of 5-18 mg·kg−1. Test for recovery was made according to the standard addition method, giving recoveries in the range of 97.6%-108%, and RSDs (n=6) of the determined values ranged from 0.30% to 4.4%. This method was used to screen 10 batches of actual samples with different matrices, and the detection rate of PBs was 40%. Methyl p-hydroxybenzoate was detected in 1 batch of samples, and ethyl p-hydroxybenzoate and propyl p-hydroxybenzoate were detected in 3 batches of samples.

       

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