中国药师
中國藥師
중국약사
CHINA PHARMACIST
2014年
4期
556-560
,共5页
钟浩%葛德洲%刘浩%邓祖磊
鐘浩%葛德洲%劉浩%鄧祖磊
종호%갈덕주%류호%산조뢰
气质联用色谱法%邻苯二甲酸酯类%口服液体制剂%塑化剂
氣質聯用色譜法%鄰苯二甲痠酯類%口服液體製劑%塑化劑
기질련용색보법%린분이갑산지류%구복액체제제%소화제
Gas chromatography tandem mass spectrometry%Phthalates%Oral liquid preparations%Plasticizer
目的：建立气相色谱-质谱联用技术同时测定口服液体制剂中16种邻苯二甲酸酯类塑化剂的检测方法。比较液-液萃取和固相萃取对液体制剂的净化效果影响,并对操作参数进行优化,建立最佳试验条件。方法：分别采用液-液萃取和固相萃取两种样品前处理方式处理样品,采用选择离子监测,以碎片的丰度比定性,外标法定量。结果：采用液-液萃取方法前处理样品时基质的干扰大,杂质峰较多,故采用固相萃取方式对样品进行前处理,GC-MS检测口服液体制剂中16中邻苯二甲酸酯类塑化剂残留量,该方法检出限为0.02μg · g-1,在0.5~8.0μg · ml-1范围内,线性良好(相关系数 r 范围0.9907~0.9998),加标回收率在71.7%~95.6%范围内,RSD为2.1%~9.7%。结论：采用固相萃取,GC-MS的方法对口服液体制剂中16中邻苯二甲酸酯类塑化剂进行检测,方法简便、快速、准确、灵敏度高,适用于口服液体制剂中16中邻苯二甲酸酯类塑化剂的测定。
目的：建立氣相色譜-質譜聯用技術同時測定口服液體製劑中16種鄰苯二甲痠酯類塑化劑的檢測方法。比較液-液萃取和固相萃取對液體製劑的淨化效果影響,併對操作參數進行優化,建立最佳試驗條件。方法：分彆採用液-液萃取和固相萃取兩種樣品前處理方式處理樣品,採用選擇離子鑑測,以碎片的豐度比定性,外標法定量。結果：採用液-液萃取方法前處理樣品時基質的榦擾大,雜質峰較多,故採用固相萃取方式對樣品進行前處理,GC-MS檢測口服液體製劑中16中鄰苯二甲痠酯類塑化劑殘留量,該方法檢齣限為0.02μg · g-1,在0.5~8.0μg · ml-1範圍內,線性良好(相關繫數 r 範圍0.9907~0.9998),加標迴收率在71.7%~95.6%範圍內,RSD為2.1%~9.7%。結論：採用固相萃取,GC-MS的方法對口服液體製劑中16中鄰苯二甲痠酯類塑化劑進行檢測,方法簡便、快速、準確、靈敏度高,適用于口服液體製劑中16中鄰苯二甲痠酯類塑化劑的測定。
목적：건립기상색보-질보련용기술동시측정구복액체제제중16충린분이갑산지류소화제적검측방법。비교액-액췌취화고상췌취대액체제제적정화효과영향,병대조작삼수진행우화,건립최가시험조건。방법：분별채용액-액췌취화고상췌취량충양품전처리방식처리양품,채용선택리자감측,이쇄편적봉도비정성,외표법정량。결과：채용액-액췌취방법전처리양품시기질적간우대,잡질봉교다,고채용고상췌취방식대양품진행전처리,GC-MS검측구복액체제제중16중린분이갑산지류소화제잔류량,해방법검출한위0.02μg · g-1,재0.5~8.0μg · ml-1범위내,선성량호(상관계수 r 범위0.9907~0.9998),가표회수솔재71.7%~95.6%범위내,RSD위2.1%~9.7%。결론：채용고상췌취,GC-MS적방법대구복액체제제중16중린분이갑산지류소화제진행검측,방법간편、쾌속、준학、령민도고,괄용우구복액체제제중16중린분이갑산지류소화제적측정。
Objective:To establish a GC-MS method for the simultaneous determination of 16 phthalate ester plasticizers in oral liquid preparations, compare the purification effect of liquid preparations by liquid-liquid extraction and solid phase extraction and opti-mize the operating parameters to determine the optimal experimental conditions. Methods:The samples were operated by liquid-liquid extraction and solid phase extraction, respectively. Selective ion monitor ( SIM) was adopt, phthalate esters were identified by the rela-tive abundance of major characteristic ions and the content was determined by an external standard method. Results:When the samples were operated by liquid-liquid extraction, the interference was strong with many impurity peaks. Therefore, the solid phase extraction was adopted for the sample pretreatment. GC-MS was used to detect the residues of 16 phthalate ester plasticizers in oral liquid prepara-tions. The detection limit was 0. 02μg·g-1 ,while the calibration curve showed good linearity within the range of 0. 25-8. 0μg·ml-1 with the correlation coefficient between 0. 990 7 and 0. 999 8. The average recoveries were 76. 0%-95. 4%. The relative standard devi-ations were between 2. 3% and 9. 6%(n=6). Conclusion: Pretreated by solid phase extraction, the residues of 16 phthalate ester plasticizers in oral liquid preparations can be detected by GC-MS with the properties of simple, fast, precise and sensitive, and it is suitable for the determination of phthalate esters in oral liquid preparations.
