CAJ | 학술논문

建立了豆芽10种植物生长调节剂的分级净化体系,采用气相色谱质谱法(GC/ MS)对该体系的效果进行了评价。豆芽先用酸性乙腈提取,浓缩后用甲醇复溶,部分经 QuECHERS 试剂盒净化后用 GC/ MS 分析2,4-D-乙酯2,4-D-丁酯。另一部分经 MCS 固相萃取柱净化,先用5 mL 甲醇洗脱得组分1,再用5%氨化甲醇洗脱得组分2；组分1浓缩后用10%三氟化硼甲醇溶液甲酯化,提取后 GC/ MS 测定4-氯苯氧乙酸、α-萘乙酸、2,4-二氯苯氧乙酸、吲哚乙酸、吲哚丁酸,组分2浓缩后用 GC/ MS 测定多效唑、激动素、6-苄基腺嘌呤。采用此净化体系对可以对不同性质的植物生长调节剂进行有效净化。结果表明,本方法完全可以用于豆芽中10种植物生长调节剂残留的检测,在豆芽中的添加0.01~0.1 mg/ kg,10种植物生长调节剂平均回收率范围为70.5%~93.2%,RSD 为5.2%~12.3%,本方法对10种植物生长调节剂的定量限(S/ N≥10)为0.01~0.025 mg/ kg,检出限(S/ N≥3)为0.003~0.008 mg/ kg。此净化体系简便、快速、准确,结合 GC/ MS 可以满足豆芽中植物生长调节剂多残留检测要求。
건립료두아10충식물생장조절제적분급정화체계,채용기상색보질보법(GC/ MS)대해체계적효과진행료평개。두아선용산성을정제취,농축후용갑순복용,부분경 QuECHERS 시제합정화후용 GC/ MS 분석2,4-D-을지2,4-D-정지。령일부분경 MCS 고상췌취주정화,선용5 mL 갑순세탈득조분1,재용5%안화갑순세탈득조분2；조분1농축후용10%삼불화붕갑순용액갑지화,제취후 GC/ MS 측정4-록분양을산、α-내을산、2,4-이록분양을산、신타을산、신타정산,조분2농축후용 GC/ MS 측정다효서、격동소、6-변기선표령。채용차정화체계대가이대불동성질적식물생장조절제진행유효정화。결과표명,본방법완전가이용우두아중10충식물생장조절제잔류적검측,재두아중적첨가0.01~0.1 mg/ kg,10충식물생장조절제평균회수솔범위위70.5%~93.2%,RSD 위5.2%~12.3%,본방법대10충식물생장조절제적정량한(S/ N≥10)위0.01~0.025 mg/ kg,검출한(S/ N≥3)위0.003~0.008 mg/ kg。차정화체계간편、쾌속、준학,결합 GC/ MS 가이만족두아중식물생장조절제다잔류검측요구。
A sequential clean-up method was developed for the quantification of 10 plant growth regulators in bean sprout by the gas chromatography / mass spectrometry (GC / MS). The analytes were firstly extracted by the acided acetonitrile. Extraction was concentrated and re-dissovled by methanol. Then, it was divided to two aliquots. One of that was analyzed for 2,4-D-butyl ester and 2,4-D-ethyl ester after the purification by QuECHERS cartridge. Another one was treated by MCS solid phase extraction column including diverse eluting steps. After eluting by 5 mL methanol, composition 1 was obtain, concentrated, and methyl esterified by 10% boron trifluoride methanol solution. The treated extract was used for the determination of 4-chlorophenoxy acetic acid, β-naphthyl acetic acid, 2,4-dichlorophenoxy acetic acid, indole acetic acid and indole butyric acid. Composition 2 collected by eluting with 5 mL 5% amonium methanol was used for the determination of paclobutrazol, Kinetin, 6-Benzylaminopurine. The clean-up procedures are designed according to different chemistry properties of these plant growth regulators. The results showed that after spiking of 0. 01-0. 1 mg / kg selected plant growth regulators, average recovery ranged from 70. 0% to 93. 2%and relative standard deviation were 5. 2% -12. 3% . Limit of quantification (LOQ S / N≥10) and limit of detection (LOD S / N≥3) were 0. 01-0. 025 mg / kg and 0. 003-0. 008 mg / kg respectively. The developed purification method is easy, fast and accurate, and can be applied to routine test of plant growth regulators in bean sprout.