市售外用抗鼻炎类凝胶产品中激素类添加物的检测及调查分析

Detection and investigation of hormone additives in external used gel products on market

目的:建立了市售抗鼻炎凝胶类产品中激素非法添加检测方法,对采集的来源于网络销售的22批次产品进行检测,并对暴露风险进行评估,提出监管建议。方法:试样中40个激素类非法添加物采用乙腈提取,高效液相色谱分离,串联质谱检测,基质外标法定量,考察测定方法学,对市售样品进行检测。结果:方法学考察试验表明,40个激素类非法添加物线性关系良好,方法精密度、重复性、回收率符合方法学要求。对市售的22批样品进行检测,总体检出阳性率为45.5%(10/22),其中械字号产品检测7批次,非法添加物检出阳性2批次,涉及非法添加倍氯米松双丙酸酯(1批次)和氯倍他索丙酸酯(1批次);消字号产品检测15批次,检出阳性8批次,涉及非法添加氯倍他索丙酸酯(7批次)和布地奈德(1批次)。结论:监测结果显示,网络销售的械字号和消字号鼻炎治疗及相关产品存在系统性的激素非法添加问题,可能产生系统性的特定人群暴露风险,亟需对网络销售的械字号和消字号鼻炎治疗及相关产品加强监管、整顿。在监测过程中检出3种激素类药物,建议加强对激素类原料药的监管。

Objective:To establish a method for detecting illegal addition of hormone in anti rhinitis gel products.Twenty-two products from online sales were tested.Exposure risks and regulatory suggestions were proposed from the monitoring results.Methods:Forty Illegal hormone additives in the sample were extracted with acetonitrile,separated by high performance liquid chromatography,detected by tandem mass spectrometry and quantified by matrix external standard method.The test methodology was evaluated and samples were determined.Results:The method showed a good linear relationship with 40 illegal hormone additives,and met the methodological requirements of precision,repeatability and recovery.Twenty-two samples were tested,and the total positive rate was 45.5%(10/22).Two in seven of medical device samples were tested positive,involving the illegal addition of beclomethasone dipropionate and clobetasopronate.Eight in fifteen hygienic samples were tested positive,including the illegal addition of clobetasopronate and budesonide.Conclusion:According to the monitoring results,there might be a systematic exposure of illegal hormone addition within the related online products,and may cause the systematic risks.It is necessary to strengthen the supervision and rectification of the rhinitis treatment and related products sold online.Meanwhile,since three kinds of hormone drugs were detected,supervision of hormone APIs should also be strengthened.