现代医药卫生
現代醫藥衛生
현대의약위생
MODERN MEDICINE HEALTH
2014年
22期
3374-3376
,共3页
余敏灵%王小林%陈文秋%封家福
餘敏靈%王小林%陳文鞦%封傢福
여민령%왕소림%진문추%봉가복
色谱法,离子交换%提取法%天花粉%二氧化硫%中草药
色譜法,離子交換%提取法%天花粉%二氧化硫%中草藥
색보법,리자교환%제취법%천화분%이양화류%중초약
Chromatography,ion exchange%Extraction%Radix trichosanthis%Sulfur dioxide%Drugs,chinese herbal
目的：建立离子色谱直接提取法测定天花粉中二氧化硫（SO2）含量的实验方法。方法采用氢氧化钾溶液（25 mmol/L）直接提取，色谱柱为AS11-HC色谱柱（4 mm×250 mm，9.0μm）；柱温20℃；淋洗液：氢氧化钾溶液（20 mmol/L）；淋洗液流速1.00 mL/min；电导检测法，电导池温度20℃通过分离度实验、精密度实验、重复性实验检测并计算分离度、亚硫酸根峰面积和天花粉中SO2含量及亚硫酸根峰面积与进样量的关系。结果亚硫酸根色谱峰与其他相邻色谱峰间有较好的分离度，峰面积变化不大，亚硫酸根平均含量为每克天花粉含SO20.1977 mg、RSD为0.6%。亚硫酸根标准溶液进样量在1.16～29.1μg（即当进样体积为100μL时，被测定溶液浓度为11.6～291.2μg/mL）与亚硫酸根色谱峰的峰面积有良好的线性关系，平均回收率为99.2%，最低定量限以被测定溶液计算为0.00138μg/mL。结论离子色谱法操作简便、准确、快速，适用于天花粉中SO2的定量检测。
目的：建立離子色譜直接提取法測定天花粉中二氧化硫（SO2）含量的實驗方法。方法採用氫氧化鉀溶液（25 mmol/L）直接提取，色譜柱為AS11-HC色譜柱（4 mm×250 mm，9.0μm）；柱溫20℃；淋洗液：氫氧化鉀溶液（20 mmol/L）；淋洗液流速1.00 mL/min；電導檢測法，電導池溫度20℃通過分離度實驗、精密度實驗、重複性實驗檢測併計算分離度、亞硫痠根峰麵積和天花粉中SO2含量及亞硫痠根峰麵積與進樣量的關繫。結果亞硫痠根色譜峰與其他相鄰色譜峰間有較好的分離度，峰麵積變化不大，亞硫痠根平均含量為每剋天花粉含SO20.1977 mg、RSD為0.6%。亞硫痠根標準溶液進樣量在1.16～29.1μg（即噹進樣體積為100μL時，被測定溶液濃度為11.6～291.2μg/mL）與亞硫痠根色譜峰的峰麵積有良好的線性關繫，平均迴收率為99.2%，最低定量限以被測定溶液計算為0.00138μg/mL。結論離子色譜法操作簡便、準確、快速，適用于天花粉中SO2的定量檢測。
목적：건립리자색보직접제취법측정천화분중이양화류（SO2）함량적실험방법。방법채용경양화갑용액（25 mmol/L）직접제취，색보주위AS11-HC색보주（4 mm×250 mm，9.0μm）；주온20℃；림세액：경양화갑용액（20 mmol/L）；림세액류속1.00 mL/min；전도검측법，전도지온도20℃통과분리도실험、정밀도실험、중복성실험검측병계산분리도、아류산근봉면적화천화분중SO2함량급아류산근봉면적여진양량적관계。결과아류산근색보봉여기타상린색보봉간유교호적분리도，봉면적변화불대，아류산근평균함량위매극천화분함SO20.1977 mg、RSD위0.6%。아류산근표준용액진양량재1.16～29.1μg（즉당진양체적위100μL시，피측정용액농도위11.6～291.2μg/mL）여아류산근색보봉적봉면적유량호적선성관계，평균회수솔위99.2%，최저정량한이피측정용액계산위0.00138μg/mL。결론리자색보법조작간편、준학、쾌속，괄용우천화분중SO2적정량검측。
Objective To establish a quantitative analysis method to determine the content of the Sulfur dioxide (SO2) in Tianhuafen by ion chromatography-direct extraction. Methods The SO2 was extracted by potassium hydroxide solution(25 mmol/L) directly with AS11-HC chromatographic column(4 mm×250 mm,9.0μm);column temperature was 20℃;eluent was potassium hydroxide solution(20 mmol/L);the flow rate of eluent was 1.00 mL/min. Conductivity detection was adopted with the conductivity temperature of 20℃. The separating degree experiment,precision experiment and repetitive test were adopted to detect and calcu-late degree of separating,peak area of sulfite,content of SO2 in each gram of Tianhuafen and the relationship between peak area and sample volume. Results The chromatographic peak of sulfite had good separating degree with its adjacent chromatographic peak,and the peak area changed little;the mean content of sulfite was 0.197 7 mg in each gram of Tianhuafen with the RSD of 0.6%. When the injection quantity of sulfite sample was in the range of 1.16-29.1μg, which meant when the injection volume of sulfite was 100μL and the concentration range of solutions was within 11.6-291.2μg/mL,there was good linear relationship be-tween the injection quantity and peak area of sulfite. The average recovery rate was 99.2%,and the limit of quantification (LOQ) was 0.00 138μg/mL. Conclusion The method of ion chromatography-direct extraction is simple,accurate,rapid and appropriate for the quantification of SO2 in Tianhuafen.
