分級凈化結合氣相色譜質譜聯用法測定豆芽中10種植物生長調節劑

吳平谷等

摘 要 建立了豆芽10種植物生長調節劑的分級凈化體系，

1 引 言

我國豆芽以作坊式生產為主，在豆芽生產過程中肆意添加植物生長調節劑催發豆芽生長常有發生，添加的植物生長調節劑主要有等。本研究針對豆芽生產過程中可能使用的10種植物生長調節劑，通過加標實驗，根據其化學性質進行分級凈化，采用氣相色譜質譜法對該凈化體系的進行了評價，獲得較好的凈化效果，有較大實際應用價值。

2 實驗部分

2.1 儀器與試劑

3.5 樣品分析

從杭州超市、農貿市場中采集豆芽各10份進行10種植物生長調節劑殘留分析，主要檢出CPA和吲哚乙酸，檢出率

分別為50%和20%，含量范圍為0.014～0.26 mg/kg，，CPA已經從GB27622011《食品安全國家標準 食品添加劑使用標準》中刪除了在豆芽生產中使用的規定。吲哚乙酸是植物內源性生長素之一，可以促進豆芽桿的生長，未見豆芽中吲哚乙酸本底含量的報道，雖然吲哚乙酸對動物的毒性較低， 目前我國尚未規定吲哚乙酸在豆芽生產中應用。

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Determination of 10 Plant Growth Regulators in Bean Sprouts by

Sequential CleaningGas ChromatographyMass Spectrometry

WU PingGu， TAN Yin， ZHANG Jin， WANG LiYuan， TANG Jun，

JIANG Wei， PAN XiaoDong， MA BingJie， NI ZhuNan， WANG TianJiao

（Zhejiang Provincial Center for Disease Control and Prevention， Hangzhou 310051， China）

Abstract A sequential cleanup 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 redissovled by methanol. Then， it was divided to two aliquots. One of that was analyzed for 2，4Dbutyl ester and 2，4Dethyl 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 4chlorophenoxy acetic acid， βnaphthyl acetic acid， 2，4dichlorophenoxy 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， 6Benzylaminopurine. The cleanup 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.

Keywords Bean sprout； Plant growth regulator； Sequential cleaning； Gas chromatographymass spectrometry

（Received 3 February 2014； accepted 17 March 2014）

吳平谷， 王 強， 沈向紅， 陳慧華， 宋國良， 應永飛， 徐小民， 趙永信.分析化學， 2008， 36（11）： 1476-1482

Determination of 10 Plant Growth Regulators in Bean Sprouts by

Sequential CleaningGas ChromatographyMass Spectrometry

WU PingGu， TAN Yin， ZHANG Jin， WANG LiYuan， TANG Jun，

JIANG Wei， PAN XiaoDong， MA BingJie， NI ZhuNan， WANG TianJiao

（Zhejiang Provincial Center for Disease Control and Prevention， Hangzhou 310051， China）

Abstract A sequential cleanup 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 redissovled by methanol. Then， it was divided to two aliquots. One of that was analyzed for 2，4Dbutyl ester and 2，4Dethyl 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 4chlorophenoxy acetic acid， βnaphthyl acetic acid， 2，4dichlorophenoxy 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， 6Benzylaminopurine. The cleanup 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.

Keywords Bean sprout； Plant growth regulator； Sequential cleaning； Gas chromatographymass spectrometry

（Received 3 February 2014； accepted 17 March 2014）

吳平谷， 王 強， 沈向紅， 陳慧華， 宋國良， 應永飛， 徐小民， 趙永信.分析化學， 2008， 36（11）： 1476-1482

Determination of 10 Plant Growth Regulators in Bean Sprouts by

Sequential CleaningGas ChromatographyMass Spectrometry

WU PingGu， TAN Yin， ZHANG Jin， WANG LiYuan， TANG Jun，

JIANG Wei， PAN XiaoDong， MA BingJie， NI ZhuNan， WANG TianJiao

（Zhejiang Provincial Center for Disease Control and Prevention， Hangzhou 310051， China）

Abstract A sequential cleanup 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 redissovled by methanol. Then， it was divided to two aliquots. One of that was analyzed for 2，4Dbutyl ester and 2，4Dethyl 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 4chlorophenoxy acetic acid， βnaphthyl acetic acid， 2，4dichlorophenoxy 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， 6Benzylaminopurine. The cleanup 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.

Keywords Bean sprout； Plant growth regulator； Sequential cleaning； Gas chromatographymass spectrometry

（Received 3 February 2014； accepted 17 March 2014）