气相色谱-负化学离子源质谱法测定聚氯乙烯塑料中的短链氯化石蜡

Determination of short chain chlorinated paraffins in polyvinyl chloride plastics by gas chromatography-negative chemical ion / mass spectrometry

建立了用于聚氯乙烯（PVC）塑料中短链氯化石蜡（SCCPs）含量测定的气相色谱-负化学离子源质谱法。采用超声萃取法对PVC塑料中的SCCPs进行萃取，萃取时间为1．5h；然后用浓硫酸法对萃取溶液进行净化处理；最后用气相色谱-质谱法在负化学电离模式、离子源温度为160℃、甲烷反应气流速为1.5mL／min等条件下对样品中的SCCPs进行定性定量分析。该方法不受样品中中链氯化石蜡（MCCPs）的干扰，可对样品中的SCCPs进行准确的定量分析。分析的12批次样品均检出SCCPs，含量在0．3×10^2-3．5×10^4mg／kg范围内。依据欧盟对SCCP的限值（196）要求，4批次样品不符合法规要求，不符合率为33．396。可见，PVC塑料具有较高的SCCPs污染风险。

A novel method was established to determine short chain chlorinated paraffms （ SC- CPs） in polyvinyl chloride （PVC） plastics by gas chromatography-negative chemical ion/mass spectrometry （GC-NCI/MS）. Ultrasonic extraction was used to extract SCCPs from PVC plas- tics. The optimal extraction time was 1.5 h, and concentrated sulfuric acid was adopted to purify the extracted solution. Finally, SCCPs in a sample were detected by GC-NCI/MS at 160 ~C and with methane reagent gas at 1.5 mL/min. This method was not influenced by medium chain chlorinated paraffms （MCCPs） in the sample, and accurate quantitation was made for SCCPs. Twelve batches of samples were analyzed and SCCPs were detected in each batch with the contents from 0. 3×10^2mg/kg to 3.5×10^4mg/kg. With respect to European limitation of SC- CPs （ 1% ）, four batches of samples did not comply with the European regulation, and they ac- counted for 33.3%. Obviously, high SCCPs risk was presented in PVC plastics.