多环芳烃（Polycyclic Aromatic Hydrocarbons,简称PAHs）是指两个以上苯环以稠环形式相连的化合物，是目前水水体、土壤中普遍存在的污染物质。PAHS具有致畸、致癌和致突变的效应，同时具有疏水性、难降解和长距离迁移等特点，导致其在环境和食品中的分布和来源引起广泛关注。
水中多环芳烃的含量一般较低，对样品的富集净化显得尤其重要。本文参考《HJ478-2009水质多环芳烃的测定 液液萃取和固相萃取高效液相色谱法》采用莱奥正压固相萃取仪对水样中16种多环芳烃进行富集、净化，气相色谱质谱仪进行检测，实现了水中16种目标物的检测分析。采用加标回收的方式进行方法验证，结果显示在1μg的加标水平下，16种多环芳烃的回收率在67.2~109.9%之间，RSD值0.9~9.1%，表明该方法具有操作简便、快速和高通量分析等优点，适合生活饮用水、地表水、地下水和海水中多环芳烃的测定。
[/fusion_text][fusion_builder_row_inner][fusion_builder_column_inner type=”1_3″ type=”1_3″ align_self=”auto” content_layout=”column” align_content=”flex-start” valign_content=”flex-start” content_wrap=”wrap” center_content=”no” column_tag=”div” target=”_self” hide_on_mobile=”small-visibility,medium-visibility,large-visibility” sticky_display=”normal,sticky” order_medium=”0″ order_small=”0″ hover_type=”none” border_style=”solid” box_shadow=”no” box_shadow_blur=”0″ box_shadow_spread=”0″ background_type=”single” gradient_start_position=”0″ gradient_end_position=”100″ gradient_type=”linear” radial_direction=”center center” linear_angle=”180″ lazy_load=”avada” background_position=”left top” background_repeat=”no-repeat” background_blend_mode=”none” background_slider_skip_lazy_loading=”no” background_slider_loop=”yes” background_slider_pause_on_hover=”no” background_slider_slideshow_speed=”5000″ background_slider_animation=”fade” background_slider_direction=”up” 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filter_sepia_hover=”0″ filter_opacity_hover=”100″ filter_blur_hover=”0″ image_id=”6065|fusion-400″ link=”https://leowlab.com/positive-pressure-solid-phase-extractor/purifier-a48/” caption_title=”Leowlab Purifier A48″ caption_text=”48位正压固相萃取仪” caption_title_transform=”capitalize” caption_text_transform=”capitalize” caption_overlay_color=”hsla(var(–awb-color7-h),var(–awb-color7-s),calc(var(–awb-color7-l) + 40%),var(–awb-color7-a))” fusion_font_variant_caption_title_font=”600″ fusion_font_family_caption_title_font=”Montserrat” caption_title_size=”16″ caption_title_color=”var(–awb-color1)” fusion_font_variant_caption_text_font=”400″ fusion_font_family_caption_text_font=”Montserrat” caption_text_size=”16″ caption_border_color=”var(–awb-color1)” caption_text_color=”var(–awb-color1)”]https://leowlab.com/wp-content/uploads/2025/10/A48-400×400.jpg[/fusion_imageframe][/fusion_builder_column_inner][fusion_builder_column_inner type=”1_3″ type=”1_3″ align_self=”auto” content_layout=”column” 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filter_hover_element=”self” filter_hue=”0″ filter_saturation=”100″ filter_brightness=”100″ filter_contrast=”100″ filter_invert=”0″ filter_sepia=”0″ filter_opacity=”100″ filter_blur=”0″ filter_hue_hover=”0″ filter_saturation_hover=”100″ filter_brightness_hover=”100″ filter_contrast_hover=”100″ filter_invert_hover=”0″ filter_sepia_hover=”0″ filter_opacity_hover=”100″ filter_blur_hover=”0″ transform_type=”regular” transform_hover_element=”self” transform_scale_x=”1″ transform_scale_y=”1″ transform_translate_x=”0″ transform_translate_y=”0″ transform_rotate=”0″ transform_skew_x=”0″ transform_skew_y=”0″ transform_scale_x_hover=”1″ transform_scale_y_hover=”1″ transform_translate_x_hover=”0″ transform_translate_y_hover=”0″ transform_rotate_hover=”0″ transform_skew_x_hover=”0″ transform_skew_y_hover=”0″ transition_duration=”300″ transition_easing=”ease” scroll_motion_devices=”small-visibility,medium-visibility,large-visibility” animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ last=”no” border_position=”all”][fusion_imageframe custom_aspect_ratio=”100″ lightbox=”no” linktarget=”_blank” align_medium=”none” align_small=”none” align=”center” hover_type=”none” magnify_duration=”120″ scroll_height=”100″ scroll_speed=”1″ caption_style=”resa” caption_align_medium=”none” caption_align_small=”none” caption_align=”center” caption_title_tag=”div” animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ hide_on_mobile=”small-visibility,medium-visibility,large-visibility” sticky_display=”normal,sticky” filter_hue=”0″ filter_saturation=”100″ filter_brightness=”100″ filter_contrast=”100″ filter_invert=”0″ filter_sepia=”0″ filter_opacity=”100″ filter_blur=”0″ filter_hue_hover=”0″ filter_saturation_hover=”100″ filter_brightness_hover=”100″ filter_contrast_hover=”100″ filter_invert_hover=”0″ filter_sepia_hover=”0″ filter_opacity_hover=”100″ filter_blur_hover=”0″ image_id=”6069|fusion-400″ link=”https://leowlab.com/nitrogen-evaporator/smartvap-ae/” caption_title=”Leowlab SmartVap AE” caption_title_transform=”capitalize” caption_text_transform=”capitalize” caption_overlay_color=”hsla(var(–awb-color7-h),var(–awb-color7-s),calc(var(–awb-color7-l) + 40%),var(–awb-color7-a))” fusion_font_variant_caption_title_font=”600″ fusion_font_family_caption_title_font=”Montserrat” caption_title_size=”16″ caption_title_color=”var(–awb-color1)” fusion_font_variant_caption_text_font=”400″ fusion_font_family_caption_text_font=”Montserrat” caption_text_size=”16″ caption_border_color=”var(–awb-color1)” caption_text=”全自动氮吹浓缩仪”]https://leowlab.com/wp-content/uploads/2025/10/QE-AE-400×400.jpg[/fusion_imageframe][/fusion_builder_column_inner][fusion_builder_column_inner type=”1_3″ type=”1_3″ align_self=”auto” content_layout=”column” align_content=”flex-start” valign_content=”flex-start” content_wrap=”wrap” center_content=”no” column_tag=”div” target=”_self” 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filter_sepia=”0″ filter_opacity=”100″ filter_blur=”0″ filter_hue_hover=”0″ filter_saturation_hover=”100″ filter_brightness_hover=”100″ filter_contrast_hover=”100″ filter_invert_hover=”0″ filter_sepia_hover=”0″ filter_opacity_hover=”100″ filter_blur_hover=”0″ transform_type=”regular” transform_hover_element=”self” transform_scale_x=”1″ transform_scale_y=”1″ transform_translate_x=”0″ transform_translate_y=”0″ transform_rotate=”0″ transform_skew_x=”0″ transform_skew_y=”0″ transform_scale_x_hover=”1″ transform_scale_y_hover=”1″ transform_translate_x_hover=”0″ transform_translate_y_hover=”0″ transform_rotate_hover=”0″ transform_skew_x_hover=”0″ transform_skew_y_hover=”0″ transition_duration=”300″ transition_easing=”ease” scroll_motion_devices=”small-visibility,medium-visibility,large-visibility” animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ last=”no” border_position=”all”][fusion_imageframe custom_aspect_ratio=”100″ lightbox=”no” linktarget=”_blank” align_medium=”none” align_small=”none” align=”center” hover_type=”none” magnify_duration=”120″ scroll_height=”100″ scroll_speed=”1″ caption_style=”resa” caption_align_medium=”none” caption_align_small=”none” caption_align=”center” caption_title_tag=”div” animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ hide_on_mobile=”small-visibility,medium-visibility,large-visibility” sticky_display=”normal,sticky” filter_hue=”0″ filter_saturation=”100″ filter_brightness=”100″ filter_contrast=”100″ filter_invert=”0″ filter_sepia=”0″ filter_opacity=”100″ filter_blur=”0″ filter_hue_hover=”0″ filter_saturation_hover=”100″ filter_brightness_hover=”100″ filter_contrast_hover=”100″ filter_invert_hover=”0″ filter_sepia_hover=”0″ filter_opacity_hover=”100″ filter_blur_hover=”0″ image_id=”6071|fusion-400″ link=”https://leowlab.com/nitrogen-generator/nitrogen-evaporator-1/clart-mp-series/” caption_title=”Leowlab NG-MP” caption_text=”氮吹用氮气发生器” caption_title_transform=”capitalize” caption_text_transform=”capitalize” caption_overlay_color=”hsla(var(–awb-color7-h),var(–awb-color7-s),calc(var(–awb-color7-l) + 40%),var(–awb-color7-a))” fusion_font_variant_caption_title_font=”600″ fusion_font_family_caption_title_font=”Montserrat” caption_title_size=”16″ caption_title_color=”var(–awb-color1)” fusion_font_variant_caption_text_font=”400″ fusion_font_family_caption_text_font=”Montserrat” caption_text_size=”16″ caption_border_color=”var(–awb-color1)”]https://leowlab.com/wp-content/uploads/2025/10/氮发-中-400×400.jpg[/fusion_imageframe][/fusion_builder_column_inner][/fusion_builder_row_inner][fusion_title title_type=”text” scroll_reveal_effect=”color_change” scroll_reveal_basis=”chars” scroll_reveal_behavior=”always” scroll_reveal_duration=”500″ scroll_reveal_stagger=”200″ scroll_reveal_delay=”0″ scroll_reveal_above_fold=”yes” marquee_direction=”left” marquee_mask_edges=”no” marquee_speed=”15000″ rotation_effect=”bounceIn” display_time=”1200″ highlight_effect=”circle” loop_animation=”once” highlight_animation_duration=”1500″ highlight_width=”9″ highlight_smudge_effect=”no” highlight_top_margin=”0″ title_link=”off” link_target=”_self” content_align=”left” size=”div” text_shadow=”no” text_shadow_blur=”0″ text_stroke=”no” text_stroke_size=”1″ text_overflow=”none” gradient_font=”no” gradient_start_position=”0″ gradient_end_position=”100″ gradient_type=”linear” radial_direction=”center center” linear_angle=”180″ style_type=”default” animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ hide_on_mobile=”small-visibility,medium-visibility,large-visibility” sticky_display=”normal,sticky” font_size=”30″ fusion_font_variant_title_font=”600″ fusion_font_family_title_font=”Montserrat” margin_bottom=”30px” margin_top=”30px”]仪器与耗材
[/fusion_title][fusion_table fusion_table_type=”2″ fusion_table_rows=”4″ fusion_table_columns=”2″ animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ hide_on_mobile=”small-visibility,medium-visibility,large-visibility”]| 前处理仪器设备 | |
|---|---|
| 萃取仪 | Leowlab Purifier A48正压固相萃取仪 |
| 浓缩系统 | Leowlab SmartVap AE全自动氮吹浓缩仪 |
| 搭配浓缩系统仪器 | Leowlab NG-MP系列氮吹用氮气发生器 |
| 分析仪器 | |
|---|---|
| 气相色谱-质谱联用仪 | 配有电子喷雾离子源（ESI） |
| 试剂及标准品 |
|---|
| 甲醇（HPLC级，CNW） |
| 乙腈（HPLC,CNW） |
| 二氯甲烷（HPLC级，CNW） |
| 氯化钠（AR级） |
| 磷酸（AR级，国药） |
| 无水硫酸钠（AR级，国药） |
| 16种多环芳烃混合溶液标准物质（200μg/ml，北方伟业计量技术研究院） |
前处理流程图
[/fusion_title][fusion_imageframe custom_aspect_ratio=”100″ lightbox=”no” linktarget=”_self” align_medium=”none” align_small=”none” align=”none” hover_type=”none” magnify_duration=”120″ scroll_height=”100″ scroll_speed=”1″ caption_style=”off” caption_align_medium=”none” caption_align_small=”none” caption_align=”none” caption_title_tag=”2″ animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ hide_on_mobile=”small-visibility,medium-visibility,large-visibility” sticky_display=”normal,sticky” filter_hue=”0″ filter_saturation=”100″ filter_brightness=”100″ filter_contrast=”100″ filter_invert=”0″ filter_sepia=”0″ filter_opacity=”100″ filter_blur=”0″ filter_hue_hover=”0″ filter_saturation_hover=”100″ filter_brightness_hover=”100″ filter_contrast_hover=”100″ filter_invert_hover=”0″ filter_sepia_hover=”0″ filter_opacity_hover=”100″ filter_blur_hover=”0″ image_id=”7414|full”]https://leowlab.com/wp-content/uploads/2026/01/多环芳烃.png[/fusion_imageframe][fusion_title title_type=”text” scroll_reveal_effect=”color_change” scroll_reveal_basis=”chars” scroll_reveal_behavior=”always” scroll_reveal_duration=”500″ scroll_reveal_stagger=”200″ scroll_reveal_delay=”0″ scroll_reveal_above_fold=”yes” marquee_direction=”left” marquee_mask_edges=”no” marquee_speed=”15000″ rotation_effect=”bounceIn” display_time=”1200″ highlight_effect=”circle” loop_animation=”once” highlight_animation_duration=”1500″ highlight_width=”9″ highlight_smudge_effect=”no” highlight_top_margin=”0″ title_link=”off” link_target=”_self” content_align=”left” size=”div” text_shadow=”no” text_shadow_blur=”0″ text_stroke=”no” text_stroke_size=”1″ text_overflow=”none” gradient_font=”no” gradient_start_position=”0″ gradient_end_position=”100″ gradient_type=”linear” radial_direction=”center center” linear_angle=”180″ style_type=”default” animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ hide_on_mobile=”small-visibility,medium-visibility,large-visibility” sticky_display=”normal,sticky” font_size=”26″ fusion_font_variant_title_font=”600″ fusion_font_family_title_font=”Montserrat” margin_bottom=”30px” margin_top=”30px”]实验步骤：
[/fusion_title][fusion_text animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ disable_idd=”no” hide_on_mobile=”small-visibility,medium-visibility,large-visibility” sticky_display=”normal,sticky” fusion_font_variant_text_font=”400″ fusion_font_family_text_font=”Montserrat” columns=”1″]标准曲线配置
采用乙腈溶剂配制浓度为 10ng/ml、20ng/ml、50ng/ml、100ng/ml 、250ng/ml的多环芳烃标准工作曲线。
样品正压固相萃取
取20ml水样（n=3），加入100μL多环芳烃中间储备液（10mg/L）和100 ml 甲醇，混合均匀。活化：固相萃取小柱分别用二氯甲烷，甲醇，超纯水，以每秒1滴的流速进行活化。上样：以每秒1滴的流速富集20ml样品。淋洗:用10mL水以10 每秒1滴速度淋洗柱子。收集：用5ml二氯甲烷浸泡C18柱，停留5min，再使用15ml二氯甲烷以每秒1滴的流速洗脱收集，并使用无水硫酸钠脱水，待GCMS分析。
LeowLab Purifier A48正压固相萃取仪条件
[/fusion_text][fusion_table fusion_table_type=”2″ fusion_table_rows=”5″ fusion_table_columns=”4″ animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ hide_on_mobile=”small-visibility,medium-visibility,large-visibility”]| SETP | 溶剂 | 体积 | 流速 |
|---|---|---|---|
| 活化 | 依次二氯甲烷、甲烷、纯水 | 各10ml | 1滴/s |
| 上样 | 水样 | 20ml | 1滴/s |
| 淋洗 | 水 | 20mL | 1滴/s |
| 洗脱 | 二氯甲烷 | 20mL | 1滴/s |
样品氮吹浓缩
用Leowlab SmartVap AE在定容到1mL，涡旋后过滤膜，转移至进样小瓶上机检测。40°C的条件下将洗脱液浓缩至约1m，然后加入3mL乙腈，继续浓缩至约 1m，加入内标后用乙腈定容到1ml，涡旋后过膜，待上机检测。
检测条件
[/fusion_text][fusion_table fusion_table_type=”2″ fusion_table_rows=”9″ fusion_table_columns=”2″ animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ hide_on_mobile=”small-visibility,medium-visibility,large-visibility”]| 条件 | 要求 |
|---|---|
| 进样口 | 290℃，不分流进样 |
| 进样体积 | 1ml |
| 色谱柱 | DB-5MS |
| 柱温 | 60℃（1min）以70℃/min速度升至120℃，以10℃/min速度升至250℃，以10℃/min速度升至280℃，以10℃/min至300℃（5min） |
| 传输线 | 280℃ |
| 流速 | 1ml/min |
| 采集方式 | SCAN&SIM |
| 质荷比 | 50-450 |
方法可行性验证
[/fusion_title][fusion_text animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ disable_idd=”no” hide_on_mobile=”small-visibility,medium-visibility,large-visibility” sticky_display=”normal,sticky” fusion_font_variant_text_font=”400″ fusion_font_family_text_font=”Montserrat” columns=”1″]为了验证该方法的回收率，本实验向污水 （20 ml）中加入上述 16 种多环芳烃的标准品品（100 μL ，10 μg/ml）进行加标回收验证（n=3）。水样加标回收率，测试结果如下表。16种PAHs 的加标回收率为 67.2~109.9%，相对标准偏差 0.9~9.1%。
[/fusion_text][fusion_table fusion_table_type=”2″ fusion_table_rows=”17″ fusion_table_columns=”7″ animation_direction=”left” animation_speed=”0.3″ animation_delay=”0″ hide_on_mobile=”small-visibility,medium-visibility,large-visibility”]| 序号 | 名称简写 | R1回收率(%) | R2回收率(%) | R3回收率(%) | AVG回收率(%) | RSD回收率(%) |
|---|---|---|---|---|---|---|
| 1 | 萘 | 113.7% | 116.3% | 98.0% | 109.3% | 9.1% |
| 2 | 苊 | 99.2% | 108.3% | 101.6% | 103.0% | 4.6% |
| 3 | 芴 | 99.2% | 97.5% | 98.5% | 98.4% | 0.9% |
| 4 | 二氢苊 | 105.5% | 109.4% | 114.7% | 109.9% | 4.2% |
| 5 | 菲 | 87.2% | 98.3% | 88.0% | 91.2% | 6.8% |
| 6 | 蒽 | 107.4% | 100.8% | 103.4% | 103.9% | 3.2% |
| 7 | 荧蒽 | 103.3% | 95.6% | 97.8% | 98.9% | 4.0% |
| 8 | 芘 | 94.3% | 97.3% | 107.4% | 99.7% | 6.9% |
| 9 | 屈 | 74.0% | 75.8% | 79.1% | 76.3% | 3.4% |
| 10 | 苯并(α)蒽 | 68.7% | 75.6% | 76.3% | 73.5% | 5.7% |
| 11 | 苯并(b)荧蒽 | 80.1% | 87.0% | 78.8% | 82.0% | 5.4% |
| 12 | 苯并(k)荧蒽 | 71.1% | 69.7% | 76.0% | 72.3% | 4.6% |
| 13 | 苯并(α)芘 | 73.2% | 80.1% | 74.6% | 76.0% | 4.8% |
| 14 | 二苯并(a,h)蒽 | 66.3% | 66.0% | 69.2% | 67.2% | 2.7% |
| 15 | 苯并(g,h,i)芘 | 71.3% | 67.3% | 74.7% | 71.1% | 5.2% |
| 16 | 茚并(1,2,3-cd)芘 | 67.5% | 70.7% | 73.8% | 70.7% | 4.5% |
2. LeowLab固相萃取仪回收率67.2~109.9%，满足实验室需求。
3. LeowLab固相萃取仪试管兼容LeowLab氮吹浓缩仪，无需样品转移，减少目标物损失。
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